Summary of the invention
High to scolder requirement while the present invention is directed to active soldering method welding CVD diamond thick-film and carbide alloy, and the shortcomings such as welding manner equipment investment is many again, technical process is complicated, welding cost is high that first diamond thick-film metallized that use at present, and the welding method of a kind of CVD diamond thick-film and carbide alloy is provided.
The present invention is achieved through the following technical solutions:
The welding method of a kind of CVD diamond thick-film and carbide alloy, first use two brightness plasma metallic cementation equipment to carry out metalized to CVD diamond thick-film aufwuchsplate, and then use same two brightness plasma metallic cementation equipment that CVD diamond thick-film aufwuchsplate and carbide alloy substrate after metallization are brazed together;
Wherein, the metallization process of CVD diamond thick-film aufwuchsplate is:
CVD diamond thick-film is carried out respectively to ultrasonic cleaning with deionized water and alcohol, with hot blast drying; CVD diamond thick-film aufwuchsplate after cleaning is placed in upward on the chip bench in the vacuum drying oven of two brightness plasma metallic cementation equipment, select the metal that can form strong carbide with carbon as target, and the distance of controlling between CVD diamond thick-film aufwuchsplate and target is 18-20mm; In the time that the vacuum drying oven of two brightness plasma metallic cementation equipment is evacuated to below 1Pa, open source electrode power supply and cathode power, pressure reduction is 250-300V, the temperature of chip bench is warming up to 700-1000 DEG C, and argon gas is as protective gas and plasma exciatiaon gas, and its flow is 60~80sccm, furnace pressure 35-65Pa, surface metalation processing time 0.5-3h, with stove cool time be 2h, finally on CVD diamond thick-film aufwuchsplate, forming thickness is the metalized coated of 2-10 μ m;
The welding procedure of CVD diamond thick-film aufwuchsplate and the soldering of carbide alloy substrate comprises the steps:
1) pretreatment process: cement carbide substrate is polished and removed surperficial oxide with sand paper, then carry out Ultrasonic Cleaning with the industrial silver soldering sheet that alcohol and acetone are 20-40 μ m to the cement carbide substrate after polishing and thickness respectively, dry up rear stand-by;
2) charging process: first place a graphite flake (prevent sample welding to chip bench) on the chip bench in the vacuum drying oven of two brightness plasma metallic cementation equipment, then order from bottom to top stacks the order of CVD diamond thick-film, scaling powder, silver soldering sheet, scaling powder, carbide alloy, finally press weight in the above, pressure is 1-2Mpa;
3) welding process: the vacuum drying oven of two brightness plasma metallic cementation equipment is evacuated to below 1Pa, heating rate with 10-20 DEG C/min is warming up to 850-900 DEG C, insulation 5-15 minute, be cooled to 500 DEG C of left and right with the speed of 5-15 DEG C/min afterwards, cool to again room temperature with the furnace, finally open stove, take out sample.
Described CVD diamond thick-film prepares by microwave plasma CVD method, heated filament CVD method or DC arc plasma CVD method.
In the metallization process of CVD diamond thick-film aufwuchsplate, described target is Ti, W, Mo, Cr, Nb, Zr, Ta or Hf.
The present invention adopts and will after the metallization of CVD diamond thick-film, weld with cement carbide substrate again, and wherein, metallization process and welding procedure can realize in same two brightness plasma metallic cementation equipment.This preparation method can overcome direct active soldering method to the too high problem of scolder requirement; And by two brightness plasma implantation techniques, metallic atom is spread at CVD diamond thick-film aufwuchsplate surface uniform, under isoionic high-temperature heating effect, form metal carbides with CVD diamond thick-film, belong between layer and CVD diamond thick-film and possess good bond strength by the incompatible guarantee fund of chemical bond; CVD diamond thick-film after metallization has surface wettability well, under the heat effect of plasma, can form with carbide alloy the welding point of high bond strength, can solve at present the conventional CVD diamond thick-film problem that welding equipment investment is many, technical process is complicated, welding cost is high that metallizes again.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described:
Embodiment 1
The welding method of a kind of CVD diamond thick-film and carbide alloy, first use two brightness plasma metallic cementation equipment to carry out metalized to CVD diamond thick-film aufwuchsplate, and then use same two brightness plasma metallic cementation equipment that CVD diamond thick-film aufwuchsplate and carbide alloy substrate after metallization are brazed together;
Wherein, the metallization process of CVD diamond thick-film aufwuchsplate is:
Prepare CVD diamond thick-film by microwave plasma CVD method, heated filament CVD method or DC arc plasma CVD method, CVD diamond thick-film is carried out respectively to ultrasonic cleaning 5min with deionized water and alcohol, with hot blast drying; CVD diamond thick-film aufwuchsplate after cleaning is placed in upward on the chip bench in the vacuum drying oven of two brightness plasma metallic cementation equipment, select and can form metal W that the purity of strong carbide is 99.9% as target with carbon, the distance between target and CVD diamond thick-film aufwuchsplate is 18mm; In the time that the vacuum drying oven of two brightness plasma metallic cementation equipment is evacuated to below 1Pa, open source electrode power supply and cathode power, source voltage 900V, cathode voltage 650V, control pressure reduction is 250V, chip bench is warming up to 900 DEG C, argon gas is as protective gas and plasma exciatiaon gas, its flow is 40sccm, furnace pressure 35Pa, workpiece temperature is 900 DEG C, surface metalation processing time 2h, with stove cool time be 2h, finally on CVD diamond thick-film aufwuchsplate, forming thickness is the metalized coated of 4 μ m;
The welding procedure of CVD diamond thick-film aufwuchsplate and the soldering of carbide alloy substrate comprises the steps:
1) pretreatment process: YG6 cement carbide substrate is polished and removed surperficial oxide with sand paper, then carry out Ultrasonic Cleaning 5min with the industrial silver soldering sheet that alcohol and acetone are 35 μ m to the cement carbide substrate after polishing and thickness respectively, dry up rear stand-by;
2) charging process: first place a graphite flake (prevent sample welding to chip bench) on the chip bench in the vacuum drying oven of two brightness plasma metallic cementation equipment, then order from bottom to top stacks the order of CVD diamond thick-film, scaling powder, silver soldering sheet, scaling powder, carbide alloy, finally press weight in the above, pressure is 2Mpa;
3) welding process: the vacuum drying oven of two brightness plasma metallic cementation equipment is evacuated to below 1Pa, is warming up to 900 DEG C with the heating rate of 20 DEG C/min, is incubated 5 minutes, be cooled to 500 DEG C with the speed of 15 DEG C/min afterwards, cool to again room temperature with the furnace, finally open stove, take out sample.
Fig. 1,2 demonstrates 900 DEG C of CVD diamond thick-film surface metalations and oozes the ESEM picture of the forward and backward surface topography of tungsten.As can be seen from Figure 2, after metalized, the metal coating on CVD diamond thick-film surface distributes continuous, fine and close.Compared with CVD diamond thick-film (Fig. 1) before metalized, CVD diamond thick-film after treatment (Fig. 2) crystal boundary becomes not obvious, but still the roughness that has had obvious polycrystal profile and keep certain, this more coarse surface is conducive to keep good bond strength after CVD diamond thick-film and the welding of carbide alloy substrate.
Fig. 3 is profile scanning Electronic Speculum picture and the EDS collection of illustrative plates that tungsten is oozed in the metallization of CVD diamond thick-film.As seen from the figure, metal coating and CVD diamond thick-film surface link together closely, appearance very close to each other, and after testing, the thickness of the tungsten coating on CVD diamond thick-film is about 4 μ m; EDS collection of illustrative plates is presented at interface W constituent content to be reduced, and C constituent content raises, and shows that the diffusion of element has occurred in interface;
In the XRD diffracting spectrum of Fig. 4, find (101) diffraction maximum and the W of faint WC
2(200) diffraction maximum of C, this shows that metal object and CVD diamond thick-film form chemical bonding under isoionic bombardment sputter and high-temperature heating effect, makes the combination that metal coating and CVD diamond thick-film can be good.
Welding result as shown in Figure 5, is carried out the demonstration of shearing test test result to welded specimen, and the shear strength of the welding point obtaining reaches 350MPa.
Embodiment 2
The welding method of a kind of CVD diamond thick-film and carbide alloy, first use two brightness plasma metallic cementation equipment to carry out metalized to CVD diamond thick-film aufwuchsplate, and then use same two brightness plasma metallic cementation equipment that CVD diamond thick-film aufwuchsplate and carbide alloy substrate after metallization are brazed together;
Wherein, the metallization process of CVD diamond thick-film aufwuchsplate is:
Prepare CVD diamond thick-film by microwave plasma CVD method, heated filament CVD method or DC arc plasma CVD method, CVD diamond thick-film is carried out respectively to ultrasonic cleaning 5min with deionized water and alcohol, with hot blast drying; CVD diamond thick-film aufwuchsplate after cleaning is placed in upward on the chip bench in the vacuum drying oven of two brightness plasma metallic cementation equipment, select the Ti that can form strong carbide with carbon as target, the distance between target and CVD diamond thick-film aufwuchsplate is 18mm; In the time that the vacuum drying oven of two brightness plasma metallic cementation equipment is evacuated to below 1Pa, open source electrode power supply and cathode power, source voltage 900V, cathode voltage 600V, control pressure reduction is 300V, chip bench is warming up to 700 DEG C, argon gas is as protective gas and plasma exciatiaon gas, its flow is 75sccm, furnace pressure 35Pa, workpiece temperature is 700 DEG C, surface metalation processing time 0.5h, with stove cool time be 2h, finally on CVD diamond thick-film aufwuchsplate, forming thickness is the metalized coated of 2 μ m;
The welding procedure of CVD diamond thick-film aufwuchsplate and the soldering of carbide alloy substrate comprises the steps:
1) pretreatment process: YG6 cement carbide substrate is polished and removed surperficial oxide with sand paper, then carry out Ultrasonic Cleaning 5min with the industrial silver soldering sheet that alcohol and acetone are 35 μ m to the cement carbide substrate after polishing and thickness respectively, dry up rear stand-by;
2) charging process: first place a graphite flake (prevent sample welding to chip bench) on the chip bench in the vacuum drying oven of two brightness plasma metallic cementation equipment, then order from bottom to top stacks the order of CVD diamond thick-film, scaling powder, silver soldering sheet, scaling powder, carbide alloy, finally press weight in the above, pressure is 2Mpa;
3) welding process: the vacuum drying oven of two brightness plasma metallic cementation equipment is evacuated to below 1Pa, is warming up to 900 DEG C with the heating rate of 20 DEG C/min, is incubated 5 minutes, be cooled to 500 DEG C with the speed of 15 DEG C/min afterwards, cool to again room temperature with the furnace, finally open stove, take out sample.
Embodiment 3
The welding method of a kind of CVD diamond thick-film and carbide alloy, first use two brightness plasma metallic cementation equipment to carry out metalized to CVD diamond thick-film aufwuchsplate, and then use same two brightness plasma metallic cementation equipment that CVD diamond thick-film aufwuchsplate and carbide alloy substrate after metallization are brazed together;
Wherein, the metallization process of CVD diamond thick-film aufwuchsplate is:
Prepare CVD diamond thick-film by microwave plasma CVD method, heated filament CVD method or DC arc plasma CVD method, CVD diamond thick-film is carried out respectively to ultrasonic cleaning 4min with deionized water and alcohol, with hot blast drying; CVD diamond thick-film aufwuchsplate after cleaning is placed in upward on the chip bench in the vacuum drying oven of two brightness plasma metallic cementation equipment, select the Zr that can form strong carbide with carbon as target, the distance between target and CVD diamond thick-film aufwuchsplate is 18mm; In the time that the vacuum drying oven of two brightness plasma metallic cementation equipment is evacuated to below 1Pa, open source electrode power supply and cathode power, source voltage 600V, cathode voltage 340V, control pressure reduction is 260V, chip bench is warming up to 900 DEG C, argon gas is as protective gas and plasma exciatiaon gas, its flow is 80sccm, furnace pressure 50Pa, workpiece temperature is 900 DEG C, surface metalation processing time 2h, with stove cool time be 2h, finally on CVD diamond thick-film aufwuchsplate, forming thickness is the metalized coated of 2 μ m;
The welding procedure of CVD diamond thick-film aufwuchsplate and the soldering of carbide alloy substrate comprises the steps:
1) pretreatment process: YG6 cement carbide substrate is polished and removed surperficial oxide with sand paper, then carry out Ultrasonic Cleaning 5min with the industrial silver soldering sheet that alcohol and acetone are 40 μ m to the cement carbide substrate after polishing and thickness respectively, dry up rear stand-by;
2) charging process: first place a graphite flake (prevent sample welding to chip bench) on the chip bench in the vacuum drying oven of two brightness plasma metallic cementation equipment, then order from bottom to top stacks the order of CVD diamond thick-film, scaling powder, silver soldering sheet, scaling powder, carbide alloy, finally press weight in the above, pressure is 1Mpa;
3) welding process: the vacuum drying oven of two brightness plasma metallic cementation equipment is evacuated to below 1Pa, is warming up to 850 DEG C with the heating rate of 18 DEG C/min, is incubated 10 minutes, be cooled to 510 DEG C with the speed of 12 DEG C/min afterwards, cool to again room temperature with the furnace, finally open stove, take out sample.
Embodiment 4
The welding method of a kind of CVD diamond thick-film and carbide alloy, first use two brightness plasma metallic cementation equipment to carry out metalized to CVD diamond thick-film aufwuchsplate, and then use same two brightness plasma metallic cementation equipment that CVD diamond thick-film aufwuchsplate and carbide alloy substrate after metallization are brazed together;
Wherein, the metallization process of CVD diamond thick-film aufwuchsplate is:
Prepare CVD diamond thick-film by microwave plasma CVD method, heated filament CVD method or DC arc plasma CVD method, CVD diamond thick-film is carried out respectively to ultrasonic cleaning 3min with deionized water and alcohol, with hot blast drying; CVD diamond thick-film aufwuchsplate after cleaning is placed in upward on the chip bench in the vacuum drying oven of two brightness plasma metallic cementation equipment, select the Hf that can form strong carbide with carbon as target, the distance between target and CVD diamond thick-film aufwuchsplate is 18mm; In the time that the vacuum drying oven of two brightness plasma metallic cementation equipment is evacuated to below 1Pa, open source electrode power supply and cathode power, source voltage 1000V, cathode voltage 710V, control pressure reduction is 290V, chip bench is warming up to 1000 DEG C, argon gas is as protective gas and plasma exciatiaon gas, its flow is 60sccm, furnace pressure 45Pa, workpiece temperature is 1000 DEG C, surface metalation processing time 2.5h, with stove cool time be 2h, finally on CVD diamond thick-film aufwuchsplate, forming thickness is the metalized coated of 8 μ m;
The welding procedure of CVD diamond thick-film aufwuchsplate and the soldering of carbide alloy substrate comprises the steps:
1) pretreatment process: YG6 cement carbide substrate is polished and removed surperficial oxide with sand paper, then carry out Ultrasonic Cleaning 5min with the industrial silver soldering sheet that alcohol and acetone are 25 μ m to the cement carbide substrate after polishing and thickness respectively, dry up rear stand-by;
2) charging process: first place a graphite flake (prevent sample welding to chip bench) on the chip bench in the vacuum drying oven of two brightness plasma metallic cementation equipment, then order from bottom to top stacks the order of CVD diamond thick-film, scaling powder, silver soldering sheet, scaling powder, carbide alloy, finally press weight in the above, pressure is 1.5Mpa;
3) welding process: the vacuum drying oven of two brightness plasma metallic cementation equipment is evacuated to below 1Pa, is warming up to 880 DEG C with the heating rate of 10 DEG C/min, is incubated 13 minutes, be cooled to 490 DEG C with the speed of 5 DEG C/min afterwards, cool to again room temperature with the furnace, finally open stove, take out sample.
Embodiment 5
The welding method of a kind of CVD diamond thick-film and carbide alloy, first use two brightness plasma metallic cementation equipment to carry out metalized to CVD diamond thick-film aufwuchsplate, and then use same two brightness plasma metallic cementation equipment that CVD diamond thick-film aufwuchsplate and carbide alloy substrate after metallization are brazed together;
Wherein, the metallization process of CVD diamond thick-film aufwuchsplate is:
Prepare CVD diamond thick-film by microwave plasma CVD method, heated filament CVD method or DC arc plasma CVD method, CVD diamond thick-film is carried out respectively to ultrasonic cleaning 5min with deionized water and alcohol, with hot blast drying; CVD diamond thick-film aufwuchsplate after cleaning is placed in upward on the chip bench in the vacuum drying oven of two brightness plasma metallic cementation equipment, select the Mo that can form strong carbide with carbon as target, the distance between target and CVD diamond thick-film aufwuchsplate is 18mm; In the time that the vacuum drying oven of two brightness plasma metallic cementation equipment is evacuated to below 1Pa, open source electrode power supply and cathode power, source voltage 700V, cathode voltage 450V, control pressure reduction is 250V, chip bench is warming up to 800 DEG C, argon gas is as protective gas and plasma exciatiaon gas, its flow is 70sccm, furnace pressure 40Pa, workpiece temperature is 800 DEG C, surface metalation processing time 3h, with stove cool time be 2h, finally on CVD diamond thick-film aufwuchsplate, forming thickness is the metalized coated of 10 μ m;
The welding procedure of CVD diamond thick-film aufwuchsplate and the soldering of carbide alloy substrate comprises the steps:
1) pretreatment process: YG6 cement carbide substrate is polished and removed surperficial oxide with sand paper, then carry out Ultrasonic Cleaning 5min with the industrial silver soldering sheet that alcohol and acetone are 20 μ m to the cement carbide substrate after polishing and thickness respectively, dry up rear stand-by;
2) charging process: first place a graphite flake (prevent sample welding to chip bench) on the chip bench in the vacuum drying oven of two brightness plasma metallic cementation equipment, then order from bottom to top stacks the order of CVD diamond thick-film, scaling powder, silver soldering sheet, scaling powder, carbide alloy, finally press weight in the above, pressure is 2Mpa;
3) welding process: the vacuum drying oven of two brightness plasma metallic cementation equipment is evacuated to below 1Pa, is warming up to 860 DEG C with the heating rate of 12 DEG C/min, is incubated 7 minutes, be cooled to 520 DEG C with the speed of 8 DEG C/min afterwards, cool to again room temperature with the furnace, finally open stove, take out sample.
Embodiment 6
The welding method of a kind of CVD diamond thick-film and carbide alloy, first use two brightness plasma metallic cementation equipment to carry out metalized to CVD diamond thick-film aufwuchsplate, and then use same two brightness plasma metallic cementation equipment that CVD diamond thick-film aufwuchsplate and carbide alloy substrate after metallization are brazed together;
Wherein, the metallization process of CVD diamond thick-film aufwuchsplate is:
Prepare CVD diamond thick-film by microwave plasma CVD method, heated filament CVD method or DC arc plasma CVD method, CVD diamond thick-film is carried out respectively to ultrasonic cleaning 4min with deionized water and alcohol, with hot blast drying; CVD diamond thick-film aufwuchsplate after cleaning is placed in upward on the chip bench in the vacuum drying oven of two brightness plasma metallic cementation equipment, select the Cr that can form strong carbide with carbon as target, the distance between target and CVD diamond thick-film aufwuchsplate is 18mm; In the time that the vacuum drying oven of two brightness plasma metallic cementation equipment is evacuated to below 1Pa, open source electrode power supply and cathode power, source voltage 800V, cathode voltage 520V, control pressure reduction is 280V, chip bench is warming up to 850 DEG C, argon gas is as protective gas and plasma exciatiaon gas, its flow is 65sccm, furnace pressure 65Pa, workpiece temperature is 850 DEG C, surface metalation processing time 1h, with stove cool time be 2h, finally on CVD diamond thick-film aufwuchsplate, forming thickness is the metalized coated of 5 μ m;
The welding procedure of CVD diamond thick-film aufwuchsplate and the soldering of carbide alloy substrate comprises the steps:
1) pretreatment process: YG6 cement carbide substrate is polished and removed surperficial oxide with sand paper, then carry out Ultrasonic Cleaning 5min with the industrial silver soldering sheet that alcohol and acetone are 30 μ m to the cement carbide substrate after polishing and thickness respectively, dry up rear stand-by;
2) charging process: first place a graphite flake (prevent sample welding to chip bench) on the chip bench in the vacuum drying oven of two brightness plasma metallic cementation equipment, then order from bottom to top stacks the order of CVD diamond thick-film, scaling powder, silver soldering sheet, scaling powder, carbide alloy, finally press weight in the above, pressure is 1Mpa;
3) welding process: the vacuum drying oven of two brightness plasma metallic cementation equipment is evacuated to below 1Pa, is warming up to 890 DEG C with the heating rate of 15 DEG C/min, is incubated 15 minutes, be cooled to 480 DEG C with the speed of 10 DEG C/min afterwards, cool to again room temperature with the furnace, finally open stove, take out sample.