CN110438457B - Modified diamond particles, modification method, application of modified diamond particles as reinforcing phase and obtained metal-based composite material - Google Patents
Modified diamond particles, modification method, application of modified diamond particles as reinforcing phase and obtained metal-based composite material Download PDFInfo
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- C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/18—Metallic material, boron or silicon on other inorganic substrates
- C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering
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- C23—COATING 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
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
- C23C14/32—Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
- C23C14/325—Electric arc evaporation
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
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- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/02—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material
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Abstract
The invention discloses modified diamond particles, a modification method, application of the modified diamond particles as a reinforcing phase and an obtained metal-based composite material, and belongs to the field of composite materials. According to the modification method of the diamond particles, the vacuum rolling coating equipment is adopted, the particles are stirred in the roller, and the coating uniformity of the diamond particles is improved; by adopting the multi-arc ion plating process, plasma is directly generated from the surface of the target material, the energy of particles attached to a matrix is high, the density of a plated film is high, and metal is easier to form carbide with diamond, so that mechanical bonding is changed into metallurgical bonding, and the interface thermal resistance can be greatly reduced; the magnetron sputtering method is adopted for coating, so that the surface of the multi-arc ion coating is improved, the surface is smoother, the fluidity of diamond particles is increased, the hot-press forming capability is improved, and the formation of pores is reduced; on the other hand, the multi-arc ion plating metal is prevented from diffusing into the base metal, so that the heat conduction performance of the base is prevented from being reduced. The coating of the modified diamond particles is compact and is not easy to fall off.
Description
Technical Field
The invention belongs to the field of composite materials, and relates to modified diamond particles, a modification method, application of the modified diamond particles as a reinforcing phase and an obtained metal-based composite material.
Background
The heat sink material for electronic packaging is developed for three generations, and cannot meet the increasing heat dissipation requirement of power devices, and the heat dissipation problem becomes a technical bottleneck of the development of the electronic information industry. The metal-based diamond composite material is a novel electronic packaging heat sink material, has excellent performances of high thermal conductivity and low thermal expansion coefficient, and becomes a research hotspot of researchers in the field as a new generation of heat sink material for electronic packaging with the most potential. Diamond is the material with the highest thermal conductivity in natural substances, which is always the hot research point of heat dissipation materials, but the price is expensive and is forbidden to researchers. With the maturity of the artificial diamond technology, the price of the artificial diamond particles gradually declines, so that the application of the diamond composite material can become practical.
According to theoretical research, the diamond particle dispersion strengthening metal matrix composite material obtained by compounding diamond serving as a second phase with a metal matrix with high heat conductivity can theoretically obtain extremely excellent heat conductivity, and the heat conductivity can theoretically reach 1000W/(m.K). However, the thermal conductivity of the metal-based diamond composite material prepared by the traditional process is only 200W/(m · K) actually, because the two phases of diamond and metal matrix have poor wettability, a method for optimizing the interface is developed, the interface bonding of the diamond and the metal matrix is improved, the interface thermal resistance between the diamond and the metal matrix is reduced, and the method becomes the core of related research work. The research finds that the ways of improving the interface combination of the two are mainly two: alloying the matrix and metalizing and modifying the surface of the diamond. In comparison, although the matrix alloying is convenient to operate and has a wide range of optional elements, the process conditions are harsh, the interface morphology and components of the alloying metal and the diamond are difficult to control, and the integrity of a carbide film is difficult to ensure; the biggest advantage of diamond surface metallization is that the appearance and the composition of a two-phase interface can be directly and effectively controlled.
There are many methods for the metallization modification of the diamond surface, the traditional process is an electroplating method, and the novel method is also a chemical vapor deposition method, a salt bath coating method, a covering combustion coating method, a vacuum micro-evaporation coating method and the like at present. However, the operation techniques of electroplating or chemical plating are relatively high, the solution ratio needs to be accurately controlled, other impurities are introduced, the combination of the plated film and the substrate is poor, and the form and the thickness of the plated film cannot be accurately controlled.
Disclosure of Invention
The invention aims to overcome the problem of poor interface bonding of metal-based diamond, and provides modified diamond particles, a modification method, application of the modified diamond particles as a reinforcing phase and an obtained metal-based composite material.
In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:
a method of modifying diamond particles comprising the steps of:
1) carrying out metallization treatment on diamond particles to generate a metal carbide and metal coating on the surfaces of the diamond particles, wherein the thickness of the coating is 100-500nm, and the metal elements in the coating are one or more of Cr, W, Ti and Zr;
2) generating a metal layer with the thickness of 5-15 mu m on the plating layer;
the step 1) and the step 2) are both carried out in vacuum rolling coating equipment.
Further, the diamond particles have a particle size of 20 to 400 μm.
Further, the metallization of the surfaces of the diamond particles in the step 1) adopts a multi-arc ion plating method.
Further, the specific process parameters of the multi-arc ion plating method are as follows: the working atmosphere is Ar, the working pressure is 0.6-1.2Pa, the arc source power is 600-1500W, the coating time is 10-30min, and the heating temperature of the vacuum chamber is 60-150 ℃.
Further, the step 2) of generating a metal layer on the metal carbide layer adopts a magnetron sputtering coating method.
Further, the specific process parameters of the magnetron sputtering coating method are as follows: the working atmosphere is Ar, the working pressure is 0.2-0.6Pa, the magnetron sputtering power is 800-1200W, the sputtering time is 50-120min, and the heating temperature of the vacuum chamber is 40-80 ℃.
Furthermore, the rotating speed of the vacuum rolling coating equipment is 10-30 r/min.
Modified diamond particles obtained by the above method for modifying diamond particles.
The modified diamond particles are used as a reinforcing phase in a metal matrix, and the element type of the metal layer is the same as that of the metal element of the metal matrix.
The metal matrix composite obtained by the above application.
Compared with the prior art, the invention has the following beneficial effects:
according to the modification method of the diamond particles, the vacuum rolling coating equipment is adopted, the particles are stirred in the roller, and the coating uniformity of the diamond particles is greatly improved; by adopting the multi-arc ion plating process, plasma is directly generated from the surface of the target material, the energy of particles attached to a matrix is high, the density of a plated film is high, and metal is easier to form carbide with diamond, so that mechanical bonding is changed into metallurgical bonding, the attachment strength is better, and the interface thermal resistance can be greatly reduced; the magnetron sputtering method is adopted for coating, so that on one hand, the surface of the multi-arc ion coating is improved, the surface is smoother, the fluidity of diamond particles is increased, the hot-press forming capability is improved, and the formation of pores is reduced; on the other hand, the multi-arc ion plating metal is prevented from diffusing into the base metal, so that the heat conduction performance of the base is prevented from being reduced. The invention adopts the multi-arc ion plating process and the magnetron sputtering process to combine the surface performance of the diamond with a double-layer film structure, thereby not only solving the problem that the diamond and the metal are not wet, but also improving the hot-press forming capability and ensuring the good heat conductivity of the matrix metal.
The modified diamond particles have flat coated surfaces, are compact and not easy to fall off, and have good wettability with a metal matrix.
The application of the modified diamond particles of the invention as a reinforcing phase in a metal matrix, the resulting composite has good thermal conductivity.
Drawings
FIG. 1 is an SEM image of Cr-plated diamond particles of a multi-arc ion plating process of example 1;
FIG. 2 is an SEM image of diamond particles after magnetron sputtering Cu plating for film coating in example 1;
FIG. 3 is an SEM image of diamond particles after plating Cr by an electroplating method;
fig. 4 is a graph of the thermal conductivity of unmodified diamond, electroplated modified diamond, and the modified diamond of example 1 after being composited with a metal as a reinforcing phase.
Detailed Description
In order to make the technical solutions of the present invention better understood, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that the terms "first," "second," and the like in the description and claims of the present invention and in the drawings described above are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used is interchangeable under appropriate circumstances such that the embodiments of the invention described herein are capable of operation in sequences other than those illustrated or described herein. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
The invention adopts the method of multi-arc ion plating and magnetron sputtering composite plating to carry out surface metallization modification on the diamond particles, and can greatly reduce the interface thermal resistance between the diamond particles and the metal matrix, thereby improving the performance of the metal-based diamond composite material as a heat sink material.
A method of modifying diamond particles comprising the steps of:
1) pretreatment of diamond particles
Putting the diamond particles into an acetone solution, cleaning for 0.5h by ultrasonic oscillation, removing hydrocarbons by cleaning, taking out, and cleaning to be neutral by using deionized water;
placing the diamond particles in 10g/L NaOH solution, cleaning for 0.5h by ultrasonic oscillation, removing oil by cleaning, taking out, and cleaning to be neutral by using deionized water;
then placing the diamond particles in HNO with the mass fraction concentration of 10 percent3And cleaning for 0.5h by ultrasonic oscillation, coarsening, taking out, and cleaning to be neutral by deionized water. Finally, the diamond particles are placed in an oven for drying.
2) Putting the diamond particles obtained in the step (1) into a roller by adopting vacuum rolling coating equipment, and ensuring that the rotating speed of the roller is 10-30r/min in the deposition process;
firstly, adopting a multi-arc ion plating process, wherein the working atmosphere is Ar, the working pressure is 0.6-1.2Pa, the arc source power is 600-1500W, the film plating time is 10-30min, and the heating temperature of a vacuum chamber is 60-150 ℃ to obtain single-layer plated diamond particles;
3) adopting a magnetron sputtering process on the surfaces of the diamond particles obtained in the step 2), wherein the working atmosphere is Ar, the working pressure is 0.2-0.6Pa, the magnetron sputtering power is 800-1200W, the sputtering time is 50-120min, and the heating temperature of a vacuum chamber is 40-80 ℃.
Example 1
Weighing 50g of diamond powder (the particle size is 100-150 mu m) by using an analytical balance, firstly putting the diamond particles into an acetone solution, cleaning for 0.5h by using ultrasonic oscillation, removing hydrocarbons by cleaning, taking out, and cleaning to be neutral by using deionized water; then placing the diamond particles in 10g/L NaOH solution, cleaning for 0.5h by ultrasonic oscillation, removing oil by cleaning, taking out, and cleaning to be neutral by using deionized water; the diamond particles were then placed in 10% HNO3Cleaning for 0.5h by ultrasonic oscillation, cleaning and coarsening, taking out, and cleaning to be neutral by deionized water; finally, the diamond particles are placed in an oven for drying.
And (3) putting the diamond particles obtained by pretreatment into a roller by adopting vacuum rolling coating equipment, and ensuring the rotating speed of the roller to be 20r/min and the vacuum degree in a vacuum chamber in the deposition process. Firstly, adopting a multi-arc ion plating method, adopting a Cr target, wherein the power is 1300W, and the plating time is 20min to obtain single-layer plated diamond particles;
and then, a magnetron sputtering method is adopted, a Cu target is adopted, the power is 1000W, the sputtering time is 70min, and the surface modified diamond particles with the double-film-layer structure are obtained.
The invention is described in further detail below with reference to the accompanying drawings:
referring to fig. 1, fig. 1 is an SEM image of Cr-plated diamond particles of the multi-arc ion plating process of example 1; as can be seen from FIG. 1, the surface of the chromium-plated diamond prepared by the method has a Cr coating which is uniformly and compactly wrapped.
Fig. 2 is an SEM image of the diamond particles after the Cu plating by the magnetron sputtering plating in example 1, and it can be seen from fig. 2 that the tungsten-plated diamond prepared by the method has a Cu plating layer with a smooth and dense surface on the surface, and the diamond particles are completely coated by the plating layer through the analysis test, and the surface is smooth and compact, and the thermal conductivity of the sintered and molded heat sink material reaches 540W/m · K.
Referring to fig. 3, fig. 3 is an SEM image of the diamond particles plated with Cr by the electroplating method, and it can be seen that the plating layer of the diamond is rough, and the particles on the plating layer are not combined into one surface, but are coral reef-shaped, and are easy to fall off during subsequent processing and use due to weak binding force, and cannot fully play the role of the plating layer.
Referring to fig. 4, fig. 4 is a graph showing thermal conductivity after non-modified diamond, electroplated modified diamond, and modified diamond of example 1 are compounded with metal as a reinforcing phase, and a volume ratio of diamond to Cu powder is 0.6: 1, the same conditions for the subsequent sintering, it can be seen that the thermal conductivity of the unmodified material is 80W/m.K, the thermal conductivity of the plating modification is 260W/m.K, and the thermal conductivity of the composite obtained in example 1 is 540W/m.K.
Tables 1 and 2 show the specific parameters of the multi-arc ion plating method and the magnetron sputtering method for plating the diamond film, respectively, the plating layer formed by the multi-arc ion plating method comprises metal carbide and metal simple substance, and the thickness distribution range of the plating layer generated in the examples 2-7 is 100-500 nm; the modified diamond obtained in examples 2 to 7 was used for magnetron sputtering, the specific parameters of which are shown in table 2, and the obtained plating layer was an upper metal layer with a thickness distribution of 5 to 15 μm.
TABLE 1 specific parameters using the Multi-arc ion plating method
TABLE 2 specific parameters using magnetron sputtering
Table 3 thermal conductivity and density values of the composites obtained in examples 2 to 7
Compared with the thermal conductivity of 80W/m.K without modification and the thermal conductivity of 260W/m.K with electroplating modification, the thermal conductivity of the compound prepared by the invention is greatly improved.
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.
Claims (8)
1. A method for modifying diamond particles, comprising the steps of:
1) carrying out metallization treatment on diamond particles to generate a metal carbide and metal coating on the surfaces of the diamond particles, wherein the thickness of the coating is 100-500nm, and the metal elements in the coating are one or more of Cr, W, Ti and Zr;
2) generating a metal layer with the thickness of 5-15 mu m on the plating layer;
the step 1) and the step 2) are both carried out in vacuum rolling coating equipment;
step 1), metallizing the surfaces of diamond particles by adopting a multi-arc ion plating method;
and 2) generating a metal layer on the coating by adopting a magnetron sputtering coating method.
2. The method for modifying diamond particles according to claim 1, wherein the diamond particles have a particle size of 20 to 400 μm.
3. The method for modifying diamond particles according to claim 1, wherein the specific process parameters of the multi-arc ion plating method are as follows: the working atmosphere is Ar, the working pressure is 0.6-1.2Pa, the arc source power is 600-1500W, the coating time is 10-30min, and the heating temperature of the vacuum chamber is 60-150 ℃.
4. The method for modifying diamond particles according to claim 1, wherein the specific process parameters of the magnetron sputtering coating method are as follows: the working atmosphere is Ar, the working pressure is 0.2-0.6Pa, the magnetron sputtering power is 800-1200W, the sputtering time is 50-120min, and the heating temperature of the vacuum chamber is 40-80 ℃.
5. The method for modifying diamond particles according to claim 1, wherein the rotation speed of the vacuum roll coating device is 10 to 30 r/min.
6. Modified diamond particles obtained by the method for modifying diamond particles according to any one of claims 1 to 5.
7. Use of modified diamond particles according to claim 6 as a reinforcing phase in a metal matrix, wherein the metal layer is of the same elemental type as the metal matrix.
8. A metal matrix composite obtained according to the use of claim 7.
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Effective date of registration: 20220608 Address after: 215000 second floor, building 3, Daxin Science Park, No. 8, Changting Road, high tech Zone, Suzhou, Jiangsu Patentee after: Suzhou Bozhi golden Diamond Technology Co.,Ltd. Address before: 710049 No. 28 West Xianning Road, Shaanxi, Xi'an Patentee before: XI'AN JIAOTONG University |