CN108315723A - The metallization process of diamond - Google Patents

The metallization process of diamond Download PDF

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Publication number
CN108315723A
CN108315723A CN201810089366.9A CN201810089366A CN108315723A CN 108315723 A CN108315723 A CN 108315723A CN 201810089366 A CN201810089366 A CN 201810089366A CN 108315723 A CN108315723 A CN 108315723A
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CN
China
Prior art keywords
diamond
layer
metallization process
film layers
composition metal
Prior art date
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Pending
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CN201810089366.9A
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Chinese (zh)
Inventor
李新宇
张学良
齐维滨
王宏
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Beijing Apollo Ding Rong Solar Technology Co Ltd
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Beijing Apollo Ding Rong Solar Technology Co Ltd
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Priority to CN201810089366.9A priority Critical patent/CN108315723A/en
Publication of CN108315723A publication Critical patent/CN108315723A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/31Coating with metals
    • C23C18/32Coating with nickel, cobalt or mixtures thereof with phosphorus or boron

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  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

The invention discloses a kind of metallization process of diamond, first by being pre-processed to diamond, then composition metal film layer is sputtered on the diamond, then nickel coating is powered in the composition metal film layer, it can complete the surface metalation processing of diamond, using the diamond after above-mentioned process, the good sealing-in with metal may be implemented, the higher welding structure of reliability is formed with metal, compared with prior art, the metallization process of the diamond of the present invention, it is more efficient, cost is lower, using the diamond of the process and the welded intensity higher of metal, the sealing-in quality of diamond and metal can be effectively improved.

Description

The metallization process of diamond
Technical field
The present invention relates to the technology field of diamond, especially a kind of metallization process of diamond.
Background technology
Diamond has the advantages that under thermal conductivity high, high mechanical strength and high frequency that dielectric properties are excellent etc., is high-frequency electromagnetic Wave carries out the preferable window material of energy transmission.
Diamond is when as frequency electromagnetic waves delivery of energy window, surface metalation and the welding quality with metal, certainly Determine the effect of its energy transmission.However, the soldering for being primarily due to diamond is poor, most of solders do not infiltrate it;Its Secondary, coefficient of thermal expansion and the metal of diamond differ greatly, and under the thermal stress effect of soldering, diamond easy tos produce micro-crack Or fracture;Finally, it is limited by diamond graphitization transition temperature, the welding of diamond and metal is also more difficult.
Therefore, it is necessary to provide a kind of metallization process of diamond, with solve diamond surface metallization and with gold The problem of belonging to welding difficulty.
Invention content
The object of the present invention is to provide a kind of metallization process of diamond, to solve diamond surface in the prior art Metallization and the problem of with metal welding difficulty, the metallization process of diamond of the invention can complete the table of diamond Face is metallized, and realizes the good welds of diamond and metal.
To achieve the goals above, the present invention provides the following technical solutions:
A kind of metallization process of diamond, includes the following steps:Diamond is pre-processed;On the diamond Sputter composition metal film layer;Nickel coating is powered in the composition metal film layer.
Preferably, pretreatment is carried out to diamond to specifically include:It polishes the surface of the diamond;Using cleaning agent ultrasound Wave cleans the diamond.
Preferably, it is specially using diamond described in cleaning agent ultrasonic cleaning:Use frequency for the super of 30kHZ-50kHZ Sound wave persistently cleans the diamond 20min-30min by cleaning agent.
Preferably, the composition metal film layer is sputtered on the diamond to specifically include:The diamond is placed on In coating machine;Ti film layers, barrier layer and soakage layer are sputtered successively from the inside to the outside on the surface of the diamond.
Preferably, on the surface of the diamond, sputtering Ti film layers, barrier layer and soakage layer specifically wrap successively from the inside to the outside It includes:The Ti film layers that sputtering thickness is 50nm-100nm on the surface of the diamond;It is sputtered in the Ti film surfaces thick Degree is the barrier layer of 200nm-250nm;The infiltration for being 250nm-300nm in barrier layer surface sputtering thickness Layer.
Preferably, the barrier layer is Mo film layers or Cu film layers or golden membranous layer.
Preferably, the soakage layer is Ni film layers.
Preferably, the Ti film layers, the barrier layer and the soakage layer are in annular shape.
Preferably, the annular width of the Ti film layers, the barrier layer and the soakage layer is 0.5mm-2mm.
Preferably, powering on nickel coating in the composition metal film layer is specially:It is thick that plating is powered in the composition metal film layer The nickel layer that the composition metal film layer is completely covered that degree is 3 μm -6 μm.
The beneficial effects of the present invention are:
The present invention provides a kind of metallization process of diamond then to exist first by being pre-processed to diamond Sputtering composition metal film layer is carried out on the diamond and powers on the operation of nickel coating in the composition metal film layer, it can be complete At the surface metalation of diamond, using the diamond of above-mentioned process, the good welds with metal may be implemented, and it is existing Technology is compared, the metallization process of diamond of the invention, metallization it is more efficient, cost is lower, and use the technique at The welding quality of the diamond of reason and the welded intensity higher of metal, diamond and metal also can effectively be changed It is kind.
Description of the drawings
Fig. 1 is the flow chart of the metallization process of the diamond of the embodiment of the present invention;
Fig. 2 is the welded schematic diagram for the diamond of the embodiment of the present invention handled using metallization process;
Fig. 3 is the structure of the diamond for measuring metallization process processing of the embodiment of the present invention and the bond strength of metal.
Reference sign:
1- diamonds, 2- weldments, 3- sealing rings, 4- aluminium oxide standard pull tension parts, 5- sheet metals.
Specific implementation mode
The embodiments described below with reference to the accompanying drawings are exemplary, is only used for explaining the present invention, and cannot be construed to Limitation of the present invention.
The present invention provides a kind of metallization process of diamond, first by being pre-processed to diamond, then in institute It states and carries out sputtering composition metal film layer on diamond and power on the operation of nickel coating in the composition metal film layer, can complete The good welds with metal may be implemented using the diamond of above-mentioned process in the surface metalation of diamond, with existing skill Art is compared, the metallization process of diamond of the invention, metallization it is more efficient, cost is lower, and use the process Diamond and metal welded intensity higher, the welding quality of diamond and metal can be also effectively improved.
As shown in Figure 1, the metallization process of diamond provided in an embodiment of the present invention, includes the following steps:
Step S01:Diamond is pre-processed;
Pretreatment is carried out to diamond to specifically include:It polishes the surface of the diamond;Using cleaning agent ultrasonic cleaning The diamond.
Wherein, generally polished by the abrasive paper for metallograph surface of the diamond is reduced with ensureing the bright and clean of diamond surface The difficulty for subsequently sputtering composition metal film layer on the diamond, improves the connection reliability of diamond and composition metal film layer.Gold Hard rock is preferably shaped to diamond diaphragm.
Preferably, it is specially using diamond described in cleaning agent ultrasonic cleaning:Use frequency for the super of 30kHZ-50kHZ Sound wave persistently cleans the diamond 20min-30min by cleaning agent.It is of course also possible to the ultrasonic wave of other frequencies is selected, Diamond is cleaned.
In a kind of specific implementation mode, the frequency of ultrasonic wave is 40kHZ, and it is 30min to continue scavenging period.
The cleaning agent can select chemical solvent, can also select the solution such as aqueous cleaning agent, such as alcohol.In ultrasonic wave After cleaning the diamond, preferably diamond is dehydrated or is dried, to shorten the time of dry diamond, improves work Efficiency.By diamond described in cleaning agent ultrasonic cleaning, the greasy dirt and impurity of diamond surface can be effectively removed.
Step S02:Composition metal film layer is sputtered on the diamond;
After pre-processing diamond, it can start to carry out metalized to diamond, first in diamond table Composition metal film layer is sputtered on face.Composition metal film layer is sputtered in diamond surface by magnetron sputtering technique, there is deposition speed Degree is fast, the preferable advantage of the combination of composition metal film layer and diamond, and can carry out essence to the thickness of composition metal film layer Really control.
Further, the composition metal film layer is sputtered on the diamond to specifically include:
The diamond is placed in coating machine;
Ti film layers, barrier layer and soakage layer are sputtered successively from the inside to the outside in the diamond surface.Ti film layers, barrier layer and The thickness range of soakage layer is preferably between 50nm-1000nm.Such as can be 50nm, 100nm, 200nm, 300nm, 500nm, 550nm, 750nm, 800nm, 880nm, 900nm, 1000nm etc., just no longer repeat one by one here.Wherein, the blocking Layer can be Mo film layers or Cu film layers or golden membranous layer.
Above-mentioned soakage layer can be Ni film layers.
More specifically, on the surface of the diamond, sputtering Ti film layers, barrier layer and soakage layer have successively from the inside to the outside Body includes:
The Ti film layers that sputtering thickness is 50nm-100nm on the surface of the diamond;
On the barrier layer that Ti film surfaces sputtering thickness is 200nm-250nm;
The soakage layer for being 250nm-300nm in barrier layer surface sputtering thickness.
Ti film layers, barrier layer and soakage layer are sputtered successively from the inside to the outside on the surface of diamond, are conducive to diamond table The characteristic in face is improved, convenient subsequently to handle the surface of diamond.Wherein, the Ti and C in diamond reacts, TiC is generated, there is TiC higher chemical stability, TiC to be covered in diamond surface, can significantly increase the surface of diamond Stability enables it with preferable binding characteristic.And the barrier layer sputtered on the outside of Ti film layers, such as Mo film layers or Cu film layers Or golden membranous layer etc., it can play the role of stopping that solder enters Ti film layers and diamond.In Mo film layers or Cu film layers or The soakage layer of the outside sputtering on the barrier layers such as golden membranous layer, soakage layer can be Ni film layers, main to play the work immersed convenient for solder With facilitating subsequent technological operation.
Preferably, the Ti film layers, the barrier layer and the infiltration film layer are in annular shape.And the Ti film layers, institute State that the region that barrier layer and the soakage layer cover is identical, area equation.
On this basis, preferably the annular width of the Ti film layers, the barrier layer and the soakage layer is sputtered to 0.5mm-2mm。
Step S03:Nickel coating is powered in the composition metal film layer.
Specifically, powering on nickel coating in the composition metal film layer is:It is 3 to power on plating thickness in the composition metal film layer μm -6 μm of the nickel layer that the composition metal film layer is completely covered.
Preferably plating mode is used to form nickel identical as its region, area equation on the surface of composition metal film layer Layer.
The electroless nickel layer on the surface of composition metal film layer, on the one hand, compared to the mode of sputtering nickel layer, generation is electroplated The yield rate of nickel layer is higher, and under the premise of obtaining the nickel layer of same thickness, and the efficiency and effect of electroless nickel layer are also more Good, on the other hand, the nickel layer of generation, which is electroplated, to carry out further protection to composition metal film layer.Using above-mentioned process Diamond, the good welds with metal may be implemented.
As shown in Fig. 2, the present invention also provides a kind of welding structure of the diamond handled using above-mentioned metallization process, packet Diamond 1 and weldment 2 are included, the weldment 2 is cylindrical in shape, and the inner wall of the weldment 2 is equipped with sealing ring 3, the Buddha's warrior attendant Stone 1 is accommodated in the weldment 2, and the diamond 1 is bonded with the sealing ring 3 and is welded to connect with the sealing ring 3.It will Diamond 1 after metallization forms such welding structure with weldment 2, is not only easier to the placement of solder, diamond 1 and welding The welding quality of part 2 is also preferable, and solder yield is also higher.
Above-mentioned welded processing technology is:Circular ring shape solder is placed first on the sealing ring 3 of weldment 2, then Diamond 1 is placed on the circular ring shape solder, then weldment 2 and diamond 1 are put into togerther in vacuum furnace, it will be true Empty heating furnace is heated near the melting temperature of circular ring shape solder, and keeps the temperature 1min-3min, is then cooled down, and is shape after cooling At above-mentioned welding structure.
On the basis of above structure, central axis of the sealing ring 3 preferably with the weldment 2.Such structure Advantageously reduce weldment 2 and welded difficulty of processing and process costs.
In addition, the present invention also provides a kind of tests to use the combination of the diamond and metal of the processing of above-mentioned metallization process strong The method of degree, includes the following steps:
Above-mentioned metallization process treated diamond will be used to form closure with sheet metal;
The closure is placed between standard pull tension part;
The closure and the standard pull tension part are welded, tension component is formed;
The tension component is fixed on tensile testing machine;
The tensile testing machine is controlled to test the bond strength of the closure.
Wherein, above-mentioned standard tensile members are preferably aluminium oxide standard pull tension part.Sheet metal is preferably copper sheet.As shown in Figure 3 For a reality of the structure of the bond strength of the diamond for testing metallization process processing and metal that are formed by the above method Example is applied, is first sealed two aluminium oxide standard pull tension parts 4 by process for sealing, and is anti-in the two aluminium oxide standards Draw and place the closure that sheet metal 5 and diamond 1 are formed between 4, in the closure 1 clamp of diamond two sheet metals 5 it Between, closure and two aluminium oxide standard pull tension parts 4 are welded in vacuum drying oven then, that is, form knot as shown in Figure 3 Structure namely tension component.Then the tension component is fixed on by fixture on tensile testing machine, then controls tensile testing machine Tension component is tested, to obtain the size of diamond 1 and the bond strength of sheet metal 5.
With the above method, measure the average bonding strength of the diamond and metal that use the processing of above-mentioned metallization process for 113.7MPa.Meet relevant criterion《SJ20600-96》It is more than the requirement of 90MPa for the bond strength of diamond and metal.From And it proves the metallization process of above-mentioned diamond and can effectively improve the bond strength of diamond and metal.
The structure, feature and effect of the present invention, the above institute are described in detail based on the embodiments shown in the drawings Only presently preferred embodiments of the present invention is stated, but the present invention is not to limit practical range, every structure according to the present invention shown in drawing Change made by thinking, or is revised as the equivalent embodiment of equivalent variations, when not going beyond the spirit of the description and the drawings, It should all be within the scope of the present invention.

Claims (10)

1. a kind of metallization process of diamond, which is characterized in that include the following steps:
Diamond is pre-processed;
Composition metal film layer is sputtered on the diamond;
Nickel coating is powered in the composition metal film layer.
2. the metallization process of diamond according to claim 1, which is characterized in that diamond pre-process specific Including:
It polishes the surface of the diamond;
Using diamond described in cleaning agent ultrasonic cleaning.
3. the metallization process of diamond according to claim 2, which is characterized in that use cleaning agent ultrasonic cleaning institute Stating diamond is specially:
It uses frequency for the ultrasonic wave of 30kHZ-50kHZ, the diamond 20min-30min is persistently cleaned by cleaning agent.
4. the metallization process of diamond according to claim 1, which is characterized in that on the diamond described in sputtering Composition metal film layer specifically includes:
The diamond is placed in coating machine;
Ti film layers, barrier layer and soakage layer are sputtered successively from the inside to the outside on the surface of the diamond.
5. the metallization process of diamond according to claim 4, which is characterized in that on the surface of the diamond by interior To sputtering Ti film layers, barrier layer and soakage layer specifically include successively outside:
The Ti film layers that sputtering thickness is 50nm-100nm on the surface of the diamond;
On the barrier layer that Ti film surfaces sputtering thickness is 200nm-250nm;
The soakage layer for being 250nm-300nm in barrier layer surface sputtering thickness.
6. the metallization process of diamond according to claim 4, which is characterized in that the barrier layer is Mo film layers or Cu Film layer or golden membranous layer.
7. the metallization process of diamond according to claim 4, which is characterized in that the soakage layer is Ni film layers.
8. the metallization process of diamond according to claim 4, which is characterized in that the Ti film layers, the barrier layer It is in annular shape with the soakage layer.
9. the metallization process of diamond according to claim 8, which is characterized in that the Ti film layers, the barrier layer Annular width with the soakage layer is 0.5mm-2mm.
10. according to the metallization process of claim 1-9 any one of them diamonds, which is characterized in that in the compound gold Belonging to electroless nickel layer in film layer is specially:
The nickel layer that the composition metal film layer is completely covered that plating thickness is 3 μm -6 μm is powered in the composition metal film layer.
CN201810089366.9A 2018-01-30 2018-01-30 The metallization process of diamond Pending CN108315723A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108517520A (en) * 2018-06-15 2018-09-11 北京铂阳顶荣光伏科技有限公司 A kind of diamond laminated film and its preparation method and application
CN110335798A (en) * 2019-06-21 2019-10-15 西安交通大学 A kind of diamond delivery of energy window and preparation method thereof

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN85100286A (en) * 1985-04-01 1986-08-27 林增栋 The technology of diamond surface metallization
CN1752267A (en) * 2005-08-18 2006-03-29 陆轻铀 Method for forming chemical combination metal plating film on diamond granules
CN102515874A (en) * 2011-12-26 2012-06-27 中国电子科技集团公司第十二研究所 Method for metalizing surface of aluminum nitride ceramic
CN102896832A (en) * 2011-07-28 2013-01-30 中国科学院金属研究所 Power module metalized ceramic substrate and metallization method thereof
CN105112754A (en) * 2015-10-12 2015-12-02 中南大学 Metal-based composite material enhanced by three-dimensional networked diamond framework as well as preparation method

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN85100286A (en) * 1985-04-01 1986-08-27 林增栋 The technology of diamond surface metallization
CN1752267A (en) * 2005-08-18 2006-03-29 陆轻铀 Method for forming chemical combination metal plating film on diamond granules
CN102896832A (en) * 2011-07-28 2013-01-30 中国科学院金属研究所 Power module metalized ceramic substrate and metallization method thereof
CN102515874A (en) * 2011-12-26 2012-06-27 中国电子科技集团公司第十二研究所 Method for metalizing surface of aluminum nitride ceramic
CN105112754A (en) * 2015-10-12 2015-12-02 中南大学 Metal-based composite material enhanced by three-dimensional networked diamond framework as well as preparation method

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108517520A (en) * 2018-06-15 2018-09-11 北京铂阳顶荣光伏科技有限公司 A kind of diamond laminated film and its preparation method and application
CN110335798A (en) * 2019-06-21 2019-10-15 西安交通大学 A kind of diamond delivery of energy window and preparation method thereof

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Application publication date: 20180724