CN105252099A - Method for welding diamond vacuum window by utilizing microwave plasma - Google Patents

Method for welding diamond vacuum window by utilizing microwave plasma Download PDF

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Publication number
CN105252099A
CN105252099A CN201510824068.6A CN201510824068A CN105252099A CN 105252099 A CN105252099 A CN 105252099A CN 201510824068 A CN201510824068 A CN 201510824068A CN 105252099 A CN105252099 A CN 105252099A
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diamond
welding
sample
microwave plasma
solder
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CN201510824068.6A
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CN105252099B (en
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马志斌
张田田
高攀
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Henan Shenzhou Lingshan New Material Co ltd
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Wuhan Institute of Technology
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K3/00Tools, devices, or special appurtenances for soldering, e.g. brazing, or unsoldering, not specially adapted for particular methods
    • B23K3/04Heating appliances
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K1/00Soldering, e.g. brazing, or unsoldering
    • B23K1/19Soldering, e.g. brazing, or unsoldering taking account of the properties of the materials to be soldered
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K2103/00Materials to be soldered, welded or cut
    • B23K2103/18Dissimilar materials

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Arc Welding In General (AREA)

Abstract

The invention relates to the field of metal and diamond welding, particularly to a method for welding a diamond vacuum window by utilizing microwave plasma. The method is characterized by comprising the following steps: S1, cleaning a metal flange and a diamond window; S2, coating the metal flange and the diamond window with solder, and contacting and stacking up surfaces coated with solder to obtain a sample; S3, putting the sample in a substrate platform in a welding cavity, vacuumizing the welding cavity, and adjusting the position of the substrate platform to enable the surface of the sample to be lower than the upper end face of a shielding cylinder; S4, enabling gas to absorb microwave energy to generate the plasma; S5, adjusting the height of the substrate platform to enable the sample to be quickly in contact with the plasma; S6, after welding, obtaining a test piece; vacuum cooling, removing vacuum, and taking out the welded test piece to complete the entire welding operation. The method remarkably improves the welding quality and stability and improves the welding efficiency of metal and diamond.

Description

A kind of method utilizing microwave plasma to weld diamond vacuum window
Technical field
The present invention relates to metal and diamond welding field, particularly relate to a kind of microwave plasma welding method, be specifically related to a kind of method utilizing microwave plasma to weld diamond vacuum window.
Technical background
Diamond is a kind of mineral be made up of carbon, is the hardest material of occurring in nature.Adamantine thermal conductivity is generally 136.16w/ (mk), thermal coefficient of expansion is minimum; Stable chemical nature, has acid resistance and alkali resistance; Also there are non magnetic, bad electric conductivity, lipophilic-hydrophobic property and frictional electricity etc., at region of ultra-red, there is good light transmission performance, therefore there is many important industrial uses, as being applied to various high power window, as high power CO 2laser window, High-Power Microwave window etc.Such as these application all need Diamond window and metal flange welding to form diamond vacuum window, are convenient to the connection with other equipment.Adamantine carbon atom has saturability and directionality, not affine with most metals, its angle of wetting is very large, chemical stability is fine, work with acid hardly, slow with alkali effect, at high temperature, diamond, when being in molten condition, can be dissolved in iron, cobalt, nickel, manganese, chromium and platinum group metal.Another group element Ti, Zr, V etc. have good compatibility with diamond, but must under uniform temperature, pressure, and are simple metal when contacting with the carbon atom of diamond surface, could generate metal carbides.Thus, diamond welds with metal the solder mostly adopted containing above-mentioned metal, and as 1958, GE added titantium hydride in Ag-Cu alloy, is realized adamantine welding by titanium.The welding method of current diamond vacuum window adopts conventional equipment and technique sintering, but above-mentioned metallic surface, at a certain temperature, is easy to oxidized, and this oxidized metal surface, can not generate metal carbide layer with diamond.If adopt vacuum or pass into the sintering furnace equipment of protective atmosphere, expensive, and temperature is slow.In the process slowly heated up, it is comparatively large that tiny solder grain can assemble change ambassador welding deformation, and seam organization is thick, and in addition, in solder, organic solvent slow releasing forms cavity, and welding quality is not good.
Microwave plasma is that the electric discharge of GAS ABSORPTION microwave energy produces plasma, the temperature of plasma changes with the microwave energy absorbed, and firing rate is fast, energy density is high, energy transformation ratio is high, pass into the oxidation that certain reducibility gas can prevent solder, be applicable to very much the welding of diamond vacuum window.At present, there is no about utilizing microwave plasma weld metal and adamantine method.The stable of microwave plasma is pressed with pass with microwave power is gentle, and the temperature of plasma with microwave power and air pressure increase and increase, if directly sample is placed directly on sparking electrode, in discharge process, the temperature of sample is slower, in solder, organic solvent can slowly make solder fluffy by some pores of volatilization generation, be unfavorable for the heat trnasfer of solder, cause the fusing of solder uneven.
Summary of the invention
In order to overcome the deficiencies in the prior art, the object of the present invention is to provide a kind of method utilizing microwave plasma to weld diamond vacuum window, the method significantly improves welding quality and stability, improves metal and adamantine welding efficiency.
For realizing goal of the invention as above, the present invention adopts technical scheme as described below:
Utilize microwave plasma to weld a method for diamond vacuum window, it is characterized in that comprising the steps:
The first step, first carries out surperficial mechanical treatment by metal flange, then metal flange and Diamond window is carried out Ultrasonic Cleaning and removes surface and oil contaminant, stand-by after dry;
Second step, metal flange after the first step being cleaned and Diamond window coat solder (coating thickness of solder is 0.03-0.5mm) respectively, then the face contact scribbling solder is stacked, applying pressure (pressure is 1-10N) makes metal flange, solder fully contacts with Diamond window, obtains sample;
3rd step, the metal flange after being stacked by second step, solder and Diamond window sample are put on the chip bench in welding chamber, then vacuumize welding chamber, regulate the position of chip bench to make sample upper surface lower than the upper surface of shielding cylinder;
4th step, passes into gas (employing hydrogen), adjusting gas flow, microwave power and air pressure, makes GAS ABSORPTION microwave energy produce plasma (i.e. microwave plasma);
5th step, regulate the position (highly) of chip bench (sample stage) to make sample enter (namely sample is 10mm apart from the distance of shielding cylinder upper surface) in microwave plasma fast, debugging welding condition ensures that solder and metal flange and Diamond window are fully wetting and combines;
6th step, after having welded, obtains test specimen; Vacuum cooled, go vacuum also to take out the test specimen welded, whole welding job completes.
In the described first step, Ultrasonic Cleaning is for carry out Ultrasonic Cleaning with acetone, alcohol solvent respectively.
Sample upper surface on chip bench in described 3rd step is 3-5mm lower than the distance of shielding cylinder upper surface.
The technological parameter that in described 4th step, microwave plasma produces is as follows: gas flow 400 ~ 1000sccm, microwave power 800-1400w, gas pressure intensity 16-25kPa.
Welding condition in described 5th step is as follows: the temperature of sample is 600-1000 DEG C, temperature retention time 1-5min.
The vacuum cooled time in described 6th step is 5-15min.
Adopt technical scheme as above, the present invention has following beneficial effect: the present invention using microwave plasma as welding thermal source, make to have suffered connection procedure time shorten (namely improving metal and adamantine welding efficiency), simple to operate, metal can weld preferably with diamond, carry out at the welding chamber of ventilation atmosphere in welding process of the present invention, avoid the impact on welding interface performance of pernicious gas in air, effectively improve weld interface combination property, microwave plasma body technique is applied to metal and welds with adamantine by the present invention, significantly improve welding quality and stability, improve metal and adamantine welding efficiency etc.
Accompanying drawing explanation
Fig. 1 is the schematic diagram that the present invention welds chamber.
In figure: 1, microwave plasma; 2, sample; 3, chip bench; 4, shielding cylinder; 5, chamber is welded.
Detailed description of the invention
Can explain the present invention in more detail by the following examples, the present invention is not limited to the following examples;
Utilize microwave plasma to weld a method for diamond vacuum window, comprise the steps:
The first step, first carries out surperficial mechanical treatment by metal flange, then metal flange and Diamond window is carried out Ultrasonic Cleaning and removes surface and oil contaminant (carrying out Ultrasonic Cleaning with acetone, alcohol solvent respectively), stand-by after dry; Because concrete metal and adamantine composition do not belong to key protection point of the present invention (Diamond window is existing), therefore will not tire out at this and state.
Second step, metal flange after the first step being cleaned and Diamond window coat solder (coating thickness of solder is 0.03-0.5mm) respectively, then the face contact scribbling solder is stacked, applying pressure (pressure is 1-10N) makes metal flange, solder fully contacts with Diamond window, obtains sample;
3rd step, metal flange after being stacked by second step, solder and Diamond window sample 2 are put on the chip bench 3 in welding chamber, then welding chamber (welding chamber) 5 is vacuumized, (specimen surface is 3-5mm lower than the distance of shielding cylinder upper surface lower than the upper surface of shielding cylinder 4 to regulate the position of chip bench to make sample upper surface, sample 2 is positioned at shielding cylinder 4, and the top of chip bench 3 is positioned at shielding cylinder 4);
4th step, passes into hydrogen, adjustments of gas (hydrogen) flow, microwave power and air pressure, makes GAS ABSORPTION microwave energy produce plasma (i.e. microwave plasma); The technological parameter that microwave plasma produces is as follows: gas flow 400 ~ 1000sccm, microwave power 800-1400w, gas pressure intensity 16-25kPa;
5th step, regulating the position of chip bench 3 to make sample 2 enter Microwave Exposure plasma 1(and sample 2 apart from the distance of shielding cylinder 4 upper surface is 10mm, now the lower surface of sample 2 is positioned on shielding cylinder 4 upper surface, shielding cylinder 4 produces microwave plasma 1 on upper surface), debugging welding condition ensures that solder and metal flange and Diamond window are fully wetting and combines; Welding condition is as follows: the temperature of sample is 600-1000 DEG C, temperature retention time 1-5min;
6th step, after having welded, obtains test specimen; Vacuum cooled (the vacuum cooled time is 5-15min), go vacuum also to take out the test specimen welded, whole welding job completes.
Weld comprehensive mechanical property is good, as shown in table 1, and in table, data are the mean value of the result of three tests.
Table 1 property of welded joint compares
Welding method Average value of shearing strength (R τMPa) Leak rate (Pam 3/s)
Microwave plasma welds 200 2.5×10 -11
Vacuum furnace welds 150 4×10 -10
With invar alloy thickness for 5mm, diameter is 25mm; Thickness of diamond is 0.3mm, and diameter is that 10mm is welded as example, and compared with prior art, welding efficiency significantly promotes in the present invention, as shown in table 2.
Table 2 welding efficiency contrast (man-hour unit, minute)
Welding method Assembly work During Welder During chief engineer
Microwave plasma welds 10 30 40
Vacuum furnace welds 10 300 310
Specific embodiments of the invention are as follows:
Embodiment 1:
Invar alloy flange thickness is 10mm, and diameter is 10mm; The thickness of Diamond window is 0.3mm, and diameter is 10mm; Solder is silver-bearing copper titanium solder.
The first step, carries out surperficial mechanical treatment by invar alloy flange, then invar alloy flange and Diamond window is used acetone, alcohol solvent ultrasonic cleaning wipe oil respectively, dried for standby.
Second step, invar alloy flange after cleaning and Diamond window surface are coated silver-bearing copper titanium solder (coating thickness of solder is 0.03-0.5mm), then the face contact scribbling silver-bearing copper titanium is stacked, applying 1-10N pressure makes invar alloy flange, silver-bearing copper titanium fully contacts with Diamond window, obtains sample;
3rd step, puts on the chip bench 3 in welding chamber by sample 2, then vacuumize welding chamber 5, regulates the position of chip bench to make sample upper surface lower than the distance 3mm of shielding cylinder upper surface;
4th step, pass into hydrogen, the gentle compression technology of adjusting gas flow, microwave power, GAS ABSORPTION microwave energy is made to produce stable plasma (microwave plasma), wherein the technological parameter of microwave plasma generation is as follows: gas flow 500sccm, microwave power 800w, gas pressure intensity 19kPa;
5th step, (namely sample 2 is 10mm apart from the distance of shielding cylinder 4 to regulate the position of chip bench to make sample Rapid contact microwave plasma, now sample 2 is positioned on shielding cylinder 4 upper surface), debugging welding condition ensures that solder and metal flange and Diamond window are fully wetting and combines, wherein welding condition is as follows: the temperature of sample 800 DEG C, temperature retention time 5min;
6th step, after having welded, obtains test specimen, and vacuum cooled (the vacuum cooled time is 5-15min), go vacuum also to take out the test specimen welded, whole welding job completes.
Almighty test machine is utilized to carry out the test of welding point shearing experiment.Leak rate measuring system is utilized to measure leak rate.Property of welded joint is as shown in table 1, and welding efficiency is as shown in table 2.
Embodiment 2:
Invar alloy flange thickness is 10mm, and diameter is 10mm; Diamond window thickness is 0.3mm, and diameter is 10mm; Solder is silver-bearing copper titanium solder.
The first step, carries out surperficial mechanical treatment by invar alloy flange, then invar alloy flange and Diamond window is used acetone, alcohol solvent ultrasonic cleaning wipe oil respectively, dried for standby.
Second step, invar alloy flange after cleaning and Diamond window surface are coated silver-bearing copper titanium solder (coating thickness of solder is 0.03-0.5mm), then the face contact scribbling silver-bearing copper titanium is stacked, applying 1-10N pressure makes invar alloy flange, silver-bearing copper titanium fully contacts with Diamond window, obtains sample;
3rd step, puts on the chip bench 3 in welding chamber by sample 2, then vacuumize welding chamber 5, regulates the position of chip bench to make sample upper surface lower than the distance 3mm of shielding cylinder upper surface;
4th step, pass into hydrogen, the gentle compression technology of adjusting gas flow, microwave power, GAS ABSORPTION microwave energy is made to produce stable plasma (microwave plasma), wherein the technological parameter of microwave plasma generation is as follows: gas flow 500sccm, microwave power 1000w, gas pressure intensity 19kPa;
5th step, (namely sample 2 is 10mm apart from the distance of shielding cylinder 4 to regulate the position of chip bench to make sample Rapid contact microwave plasma, now sample 2 is positioned on shielding cylinder 4 upper surface), debugging welding condition ensures that solder and metal flange and Diamond window are fully wetting and combines, wherein welding condition is as follows: the temperature of sample 900 DEG C, temperature retention time 4min;
6th step, after having welded, obtains test specimen, and vacuum cooled (the vacuum cooled time is 5-15min), go vacuum also to take out the test specimen welded, whole welding job completes.
Almighty test machine is utilized to carry out the test of welding point shearing experiment.Leak rate measuring system is utilized to measure leak rate.Property of welded joint is as shown in table 1, and welding efficiency is as shown in table 2.
Embodiment 3:
Invar alloy flange thickness is 10mm, and diameter is 10mm; Diamond window thickness is 0.3mm, and diameter is 10mm; Solder is silver-bearing copper titanium solder.
The first step, carries out surperficial mechanical treatment by invar alloy flange, then invar alloy flange and Diamond window is used acetone, alcohol solvent ultrasonic cleaning wipe oil respectively, dried for standby.
Second step, invar alloy flange after cleaning and Diamond window surface are coated silver-bearing copper titanium solder (coating thickness of solder is 0.03-0.5mm), then the face contact scribbling silver-bearing copper titanium is stacked, applying 1-10N pressure makes invar alloy flange, silver-bearing copper titanium fully contacts with Diamond window, obtains sample;
3rd step, puts on the chip bench 3 in welding chamber by sample 2, then vacuumize welding chamber 5, regulates the position of chip bench to make sample upper surface lower than the distance 3mm of shielding cylinder upper surface;
4th step, pass into hydrogen, the gentle compression technology of adjusting gas flow, microwave power, GAS ABSORPTION microwave energy is made to produce stable plasma (microwave plasma), wherein the technological parameter of microwave plasma generation is as follows: gas flow 500sccm, microwave power 1300w, gas pressure intensity 19kPa;
5th step, (namely sample 2 is 10mm apart from the distance of shielding cylinder 4 to regulate the position (sample rising) of chip bench to make sample Rapid contact microwave plasma, now sample 2 is positioned on shielding cylinder 4 upper surface), debugging welding condition ensures that solder and metal flange and Diamond window are fully wetting and combines, wherein welding condition is as follows: the temperature of sample 1000 DEG C, temperature retention time 3min;
6th step, after having welded, obtains test specimen, and vacuum cooled (the vacuum cooled time is 5-15min), go vacuum also to take out the test specimen welded, whole welding job completes.
Almighty test machine is utilized to carry out the test of welding point shearing experiment.Leak rate measuring system is utilized to measure leak rate.Property of welded joint is as shown in table 1, and welding efficiency is as shown in table 2.
The bound of each raw material of the present invention, interval value, and the bound of technological parameter (as gas flow, microwave power, gas pressure intensity etc.), interval value can realize the present invention, do not enumerate embodiment at this.
The embodiment selected in the present invention in order to open object of the present invention, currently thinks to be suitable for, but it is to be understood that the present invention is intended to comprise all changes belonging to the embodiment in this design and invention scope and improvement.。

Claims (6)

1. utilize microwave plasma to weld a method for diamond vacuum window, it is characterized in that comprising the steps:
The first step, first carries out surperficial mechanical treatment by metal flange, then metal flange and Diamond window is carried out Ultrasonic Cleaning and removes surface and oil contaminant, stand-by after dry;
Second step, the metal flange after the first step being cleaned and Diamond window coat solder respectively, and then contacted in the face scribbling solder and stack, applying pressure makes metal flange, solder fully contacts with Diamond window, obtains sample;
3rd step, the metal flange after being stacked by second step, solder and Diamond window sample are put on the chip bench in welding chamber, then vacuumize welding chamber, regulate the position of chip bench to make sample upper surface lower than the upper surface of shielding cylinder;
4th step, passes into gas, adjusting gas flow, microwave power and air pressure, makes GAS ABSORPTION microwave energy produce plasma;
5th step, regulates the position of chip bench to make sample Rapid contact microwave plasma, and debugging welding condition ensures that solder and metal flange and Diamond window are fully wetting and combines;
6th step, after having welded, obtains test specimen; Vacuum cooled, go vacuum also to take out the test specimen welded, whole welding job completes.
2. a kind of method utilizing microwave plasma to weld diamond vacuum window according to claim 1, is characterized in that: in the described first step, Ultrasonic Cleaning is for carry out Ultrasonic Cleaning with acetone, alcohol solvent respectively.
3. a kind of method utilizing microwave plasma to weld diamond vacuum window according to claim 1, is characterized in that: the sample upper surface on the chip bench in described 3rd step is 3-5mm lower than the distance of shielding cylinder upper surface.
4. a kind of method utilizing microwave plasma to weld diamond vacuum window according to claim 1, it is characterized in that: the technological parameter that in described 4th step, microwave plasma produces is as follows: gas flow 400 ~ 1000sccm, microwave power 800-1400W, gas pressure intensity 16-25kPa.
5. a kind of method utilizing microwave plasma to weld diamond vacuum window according to claim 1, is characterized in that: the welding condition in described 5th step is as follows: the temperature of sample is 600-1000 DEG C, temperature retention time 1-5min.
6. a kind of method utilizing microwave plasma to weld diamond vacuum window according to claim 1, is characterized in that: the vacuum cooled time in described 6th step is 5-15min.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107546109A (en) * 2017-08-31 2018-01-05 武汉工程大学 A kind of method for the surface carborundum that the Diamond window prepared on a silicon substrate is removed using hydrogen plasma
CN108336153A (en) * 2017-12-29 2018-07-27 长沙新材料产业研究院有限公司 A kind of Diamond window air locking and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5499754A (en) * 1993-11-19 1996-03-19 Mcnc Fluxless soldering sample pretreating system
JPH08281423A (en) * 1995-04-07 1996-10-29 Tamura Seisakusho Co Ltd Method and equipment for fluxless soldering
US20100193574A1 (en) * 2009-01-30 2010-08-05 General Electric Company Microwave brazing process and assemblies and materials therefor
CN103894695A (en) * 2014-04-22 2014-07-02 太原理工大学 Method for welding CVD diamond thick film and hard alloy

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5499754A (en) * 1993-11-19 1996-03-19 Mcnc Fluxless soldering sample pretreating system
JPH08281423A (en) * 1995-04-07 1996-10-29 Tamura Seisakusho Co Ltd Method and equipment for fluxless soldering
US20100193574A1 (en) * 2009-01-30 2010-08-05 General Electric Company Microwave brazing process and assemblies and materials therefor
CN103894695A (en) * 2014-04-22 2014-07-02 太原理工大学 Method for welding CVD diamond thick film and hard alloy

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107546109A (en) * 2017-08-31 2018-01-05 武汉工程大学 A kind of method for the surface carborundum that the Diamond window prepared on a silicon substrate is removed using hydrogen plasma
CN107546109B (en) * 2017-08-31 2019-12-17 武汉工程大学 Method for removing silicon carbide on surface of diamond window prepared on silicon substrate by using hydrogen plasma
CN108336153A (en) * 2017-12-29 2018-07-27 长沙新材料产业研究院有限公司 A kind of Diamond window air locking and preparation method thereof
CN108336153B (en) * 2017-12-29 2020-07-17 长沙新材料产业研究院有限公司 Diamond window sealing device and preparation method thereof

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