CN111250715A - Three-dimensional MEMS structure metal filling method based on powder sintering process - Google Patents
Three-dimensional MEMS structure metal filling method based on powder sintering process Download PDFInfo
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- CN111250715A CN111250715A CN202010153051.3A CN202010153051A CN111250715A CN 111250715 A CN111250715 A CN 111250715A CN 202010153051 A CN202010153051 A CN 202010153051A CN 111250715 A CN111250715 A CN 111250715A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
- B22F7/06—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools
- B22F7/08—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools with one or more parts not made from powder
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
- B22F3/093—Compacting only using vibrations or friction
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81B—MICROSTRUCTURAL DEVICES OR SYSTEMS, e.g. MICROMECHANICAL DEVICES
- B81B7/00—Microstructural systems; Auxiliary parts of microstructural devices or systems
- B81B7/02—Microstructural systems; Auxiliary parts of microstructural devices or systems containing distinct electrical or optical devices of particular relevance for their function, e.g. microelectro-mechanical systems [MEMS]
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/70—Manufacture or treatment of devices consisting of a plurality of solid state components formed in or on a common substrate or of parts thereof; Manufacture of integrated circuit devices or of parts thereof
- H01L21/71—Manufacture of specific parts of devices defined in group H01L21/70
- H01L21/768—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics
- H01L21/76838—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics characterised by the formation and the after-treatment of the conductors
- H01L21/76877—Filling of holes, grooves or trenches, e.g. vias, with conductive material
Abstract
The invention discloses a three-dimensional MEMS structure metal filling method based on a powder sintering process, which belongs to the field of high-precision electronics. Meanwhile, the process is simple, the time is greatly shortened compared with the traditional electroplating process, the efficiency is improved, and the method is suitable for batch production and further improves the productivity; the invention has smaller requirements on the shape of the structure, particularly the depth-to-width ratio, can be flexibly applied to the high depth-to-width ratio structure which can not be realized by electroplating, and improves the compatibility.
Description
Technical Field
The invention relates to the field of high-precision electronics, in particular to a three-dimensional MEMS structure metal filling method based on a powder sintering process.
Background
Micro-Electro-Mechanical systems (MEMS), also called Micro-Electro-Mechanical systems, microsystems, micromachines, etc., refer to high-tech devices with dimensions of a few millimeters or even smaller. The internal structure of the micro-electro-mechanical system is generally in the micron or even nanometer scale, and the micro-electro-mechanical system is an independent intelligent system. The MEMS process has the characteristics of high precision, small size, suitability for batch production and the like, and is widely used in high-precision electronic mechanical equipment, and the three-dimensional MEMS structure can more fully utilize the space in the vertical direction of the substrate, so that the power density of the device is improved, and therefore, the step of improving the energy efficiency is realized by realizing electrical interconnection in the MEMS structure, particularly in the vertical direction.
At present, the metal filling method for realizing electrical interconnection is mainly electroplating.
Copper has good electrical and thermal properties and high yield, and is an ideal material for electroplating. The through hole electroplating of copper utilizes the principle of electrolytic chemical reaction, anode metal loses electrons and becomes metal ions, the ions are driven by current provided by a power supply, the ions move to a cathode in electroplating solution to obtain electrons and become metal simple substances, and the electrons are finally attached to the surface of the cathode to accumulate and grow in the through hole to finish filling. Generally, a plating circuit comprises a plating power supply, a lead, a cathode, an anode, a plating solution and the like, and the working principle of the plating circuit is shown in FIG. 1.
The current plating liquid mainly includes ionic compounds (containing metal ions to be attached), halogen ionic compounds (usually sodium chloride), pH stabilizers (sulfuric acid), and additives (organic substances). When the current is switched on, after the experiment begins, under the action of the potential difference between the anode plate and the cathode plate: metal ions (cations) move to the cathode to carry out reduction reaction to form a metal simple substance; while the metal of the anode dissolves into metal ions into the plating solution to maintain the concentration of the metal ions. (Tangjun. copper electroplating fill in through-silicon vias (TSV) and electrochemical behavior research [ D ]. university of Chinese academy of sciences 2015)
The technique is more complete in surface plating in the horizontal direction, and can achieve more uniform and rapid filling, while structures in the vertical direction, especially with higher aspect ratios, are more severely affected by the rate, thereby reducing efficiency.
In 2012, he latte nan et al (lie anethole, zeia, wangdjun, wang modesty,&the method comprises the following steps of (2012) Wei, optimization research of a through silicon via electroplating copper filling process, special equipment for the electronic industry, 41(10), 6-10), and complete filling of the through silicon via with the aperture of 40 mu m and the hole depth of 180 mu m by improving electroplating process conditions. The conventional through hole electroplating filling process is adopted, silicon-based structure etching is carried out in sequence, an insulating layer and a seed layer are deposited, and an experimental process of electroplating growth metal is started. They first investigated the effect of different current densities on copper filling by varying the plating current density and determined the optimum current density to be 1A/dm2. Under the same experimental conditions, the influence of different treatments before electroplating, such as ultrasonic cleaning, deionized water rinsing, vacuum pretreatment and the like, on the filling effect is studied in detail. Experiments show that compared with the mode of ultrasonic cleaning and deionized water flushing, the vacuum pretreatment can effectively remove air bubbles in through holes of the silicon wafer without damaging the seed layer structure, so that a better filling effect can be obtained, and finally the effect of the filling rate approximate to 100% can be achieved, as shown in fig. 2.
In 2015, Chuang et al (Chuang, H.C., Li, H.F., Lin, Y.S., Lin, Y.H.,&Huang,C.S.(2013).The development of an atom chip with through silicon vias for an ultra-high-vacuum cell.Journal of Micromechanicsµengineering,23(23),085004.) innovatively uses a supercritical carbon dioxide electrolyte solution as an electroplating solution, combines a vacuum pretreatment process, and adopts 3A/dm2The direct current is used for electroplating, so that the silicon through hole with the depth of 525 mu m and the width of 70 mu m is filled without gaps, as shown in figure 3; the conventional process comprises through hole etching, thermal oxidation to form an insulating layer, seed layer sputtering, through hole electroplating filling and the like. Due to the large amount of carbon dioxideThe solution is dissolved in the electrolyte solution, the affinity between the solution and the side wall of the through hole is obviously improved, and the infiltration effect is effectively enhanced. In the experiment, a good experiment effect can be obtained without additives, but the arrangement of through holes on the silicon wafer to be plated is sparse, the filling speed difference of the through holes is large, and all the holes need to be full of copper in a mode of covering an adhesive tape although complete filling is realized.
In 2019, Li et al (Li Haiwang, Liu Jiansi, Xu Tiantong, Xia Junchhao, Tan Xiao, Tao Zhi. the creation and Optimization of High Aspect Ratio Through-Silicon-video electroreproduction for 3D indicator) [ J]Micromachines,2018,9(10), electroplating solutions with different additive concentrations were prepared using a pulsed power supply as the experimental power supply, and the process flow is shown in fig. 4. The optimization method is determined by the designed control variable experiment. In the control variable experiment, the system analyzes the relationship among various experimental variables such as current density, additive concentration, TSV with different shapes and the like. The influence of different factors on the experimental result and the optimization parameters are determined by considering the electroplating speed and the quality. The results show that increasing the current density increases the plating rate but decreases the plating quality. The additive works well, while its concentration is controlled within a suitable range. The shape of the TSV also affects the plating results. When the current density is 1.5A/dm2And when the concentration of the additive is 1ml/l, the TSV filtering effect is relatively good. Under optimized parameters, the TSV with the depth of 500-microns and the height-to-width ratio of 10:1 is completely filled in 20 hours, and the density of the through holes reaches 70/mm2. Finally, the parameters were optimized to complete a 1000-micron depth electrochemical process of 100 micron diameter in 45 hours, which is the deepest and smallest step to successfully fabricate three-dimensional inductors to date.
However, the electroplating filling schemes shown in fig. 1 and fig. 2 cannot achieve a high aspect ratio, the size of the device in the vertical direction is greatly limited, and the compatibility is not high. The electroplating technique shown in FIG. 3 achieves a high aspect ratio (10:1), but takes too long (1000 μm/45 hours).
As can be seen from the above, the more common electroplating techniques have several obvious disadvantages:
1. the instability of the wet environment of the plating solution may affect the device, and once bubbles possibly occurring in the plating process enter the structure, the effect of electrical connection is inevitably affected; 2. the structure size has certain requirements, and high depth-to-width ratio filling is difficult to realize; 3. it takes a long time and mass production is difficult to achieve. The electroplating speed is as fast as 1000 mu m/45h, which greatly reduces the production efficiency.
Disclosure of Invention
In view of the above, the present invention provides a new method for realizing metal filling of a three-dimensional MEMS structure, that is, a three-dimensional MEMS structure metal filling method based on powder sintering, which improves production efficiency, provides a more stable dry environment, and is suitable for a high aspect ratio MEMS microstructure.
In order to achieve the above purpose, the invention provides the following technical scheme:
the invention discloses a powder sintering-based metal filling method for a three-dimensional MEMS structure, which comprises the step of sintering the three-dimensional MEMS structure in a protective gas atmosphere after metal powder is filled in the three-dimensional MEMS structure.
Preferably, the metal powder is pre-alloyed powder of copper-tin alloy, copper-aluminum alloy or copper-zinc alloy.
Preferably, the copper-tin alloy prealloyed powder has a copper-tin volume ratio of 1:1, average particle size 15 μm.
Preferably, the protective gas is an inert gas.
Preferably, the inert gas is nitrogen or argon.
Preferably, the concentration of the nitrogen is 90-100%.
Preferably, the protective gas further comprises a reducing gas.
Preferably, the reducing gas is hydrogen or carbon monoxide.
Preferably, the concentration of hydrogen is less than 10%.
Specifically, the metal filling method for the three-dimensional MEMS structure based on powder sintering includes the following steps:
firstly, pre-laying metal powder in a fixture with an upper through groove;
step (2) placing the test piece on the powder;
pouring metal powder into the clamp through the through groove until the metal powder covers the test piece, and placing the test piece on a vibration table for vibration;
removing powder on the upper surface after fully vibrating;
repeating the pouring and vibrating steps for 2-3 times;
step (6), placing the clamp filled with the metal powder and the test piece in a high-temperature annealing furnace, and sintering in a protective gas atmosphere;
step (7), completing sintering, and separating the clamp;
and (8) taking out a sample, and thinning and polishing to obtain the complete three-dimensional MEMS structure.
Compared with the prior art, the powder sintering-based metal filling method for the three-dimensional MEMS structure has the beneficial effects that:
the method has the advantages that the step of sintering is carried out under the protective gas atmosphere after the three-dimensional MEMS structure is filled with metal powder, no liquid environment exists in the whole technological process, the influence of instability of liquid and generation of bubbles on the micron-scale structure is avoided to the greatest extent, and the filling effect is good. Meanwhile, the process is simple, the time is greatly shortened compared with the traditional electroplating process, the efficiency is improved, and the method is suitable for batch production and further improves the productivity; the invention has smaller requirements on the shape of the structure, particularly the depth-to-width ratio, can be flexibly applied to the high depth-to-width ratio structure which can not be realized by electroplating, and improves the compatibility.
Drawings
In order to more clearly illustrate the embodiments of the present application or technical solutions in the prior art, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments described in the present invention, and other drawings can be obtained by those skilled in the art according to the drawings.
FIG. 1 is a schematic diagram of electrolytic plating.
FIG. 2 is a graph showing the effect of copper filling under vacuum pretreatment.
FIG. 3 is a graph showing the plating effect of the supercritical carbon dioxide plating solution.
Fig. 4 is a via fill mode mechanism.
FIG. 5 is an effect diagram of the test piece before filling according to the embodiment of the present invention.
Fig. 6 is a schematic view of a structure of a clamp according to an embodiment of the present invention.
FIG. 7 is a process flow diagram of an embodiment of the present invention.
FIG. 8 is a diagram illustrating the effects of the filled test pieces according to the embodiment of the present invention.
FIG. 9 is a diagram of a sintered product of a test piece according to an embodiment of the present invention.
Fig. 10-15 are SEM images of samples after removal of the silicon substrate after pack-sintering in accordance with embodiments of the present invention.
Detailed Description
The invention discloses a powder sintering-based metal filling method for a three-dimensional MEMS structure, which comprises the step of sintering the three-dimensional MEMS structure in a protective gas atmosphere after metal powder is filled in the three-dimensional MEMS structure.
Wherein the metal powder is pre-alloyed powder of copper-tin alloy, copper-aluminum alloy or copper-zinc alloy. The high-pressure atomization method for prealloying powder is characterized by that according to the designed matrix proportion, the metals with various components are smelted into alloy in advance before sintering, then atomized and sprayed to obtain the matrix powder with required grain size, and the different components can be combined together before filling so as to radically prevent segregation. Preferably, the copper-tin alloy prealloyed powder has a copper-tin volume ratio of 1:1, average particle size 15 μm, spherical. The powder proportioning aims at reducing the melting point of target metal (Cu), mixed tin is common, copper-aluminum alloy and copper-zinc alloy can be used as filling materials, and the proportioning can be compared with the melting point of an alloy phase diagram. The sintering temperature and the test piece are related to the properties of the metal powder used, generally around the melting point of the metal powder.
In order to make the technical solutions of the present invention better understood by those skilled in the art, the present invention will be further described in detail with reference to the accompanying drawings and examples.
The method takes a three-dimensional spiral inductor with the wire diameter of 100 mu m and the height of 1000 mu m as a sample, and the highest aspect ratio reaches 10:1 as shown in figure 5 before filling. The sample material used was silicon, which had a melting point above 1400 ℃ and well above the metal powder (650 ℃).
The clamp used in the present invention is designed as a double layer clamp as shown in fig. 6. The clamp is made of high-temperature-resistant and flat-surface materials such as quartz glass. The upper strata is a little higher than the structure that has logical groove of test piece, and the lower floor is the bottom plate. The two layers are bonded in alignment during use in order to facilitate release of the structure after sintering the two layers apart. The adhesive can be made by coating high-temperature resistant silica gel on a substrate of a specially processed high-temperature resistant insulating material Polyimide Film (Polyimide Film) by adopting Polyimide TAPE (KAPTON TAPE), has super high-temperature resistance and is convenient to operate and remove.
The protective gas in this embodiment is a mixture of hydrogen and nitrogen, and the ratio of the synthetic gas (Forming gas) may vary, and the synthetic gas is also called dissociated ammonia protective gas and is often used as a protective gas during annealing due to the following reaction that generates the synthetic gas, and the hydrogen ratio is recommended here to be less than 10%.
The specific process steps of the method of the present invention are shown in fig. 7.
Firstly, pre-laying metal powder in a fixture with an upper through groove;
step (2) placing the test piece on the powder;
pouring metal powder into the clamp through the through groove until the metal powder covers the test piece, and placing the test piece on a vibration table for vibration; the vibration frequency is related to the filling structure and the powder property, generally, 20-50 Hz is adopted for the metal powder with the micron magnitude, and the metal powder can be layered after 2-4 minutes, the powder is layered due to the overhigh vibration frequency, the powder distribution area is stable due to the lengthening of the vibration time, and the influence of continuous vibration on the filling effect is small after the balance is achieved. The structure of the embodiment adopts 40Hz and 120 s;
removing powder on the upper surface after fully vibrating;
repeating the pouring and vibrating steps for 2-3 times, and fully filling, as shown in fig. 8;
step (6), placing the clamp filled with the metal powder and the test piece in a high-temperature annealing furnace, and sintering in a protective gas atmosphere; in this example, copper-tin prealloyed powder with a 1:1 volume ratio is used, with a melting point of about 650 ℃, so the sintering procedure used is 20 ℃ 3h-700 ℃ 1h-800 ℃ 1h-800 ℃ 4h-20 ℃, with 95% nitrogen and 5% hydrogen as the protective gas.
Step (7), completing sintering, and separating the clamp;
and (8) taking out a sample, grinding and polishing to obtain a complete three-dimensional MEMS structure, wherein a finished product after sintering is shown in figure 9.
The invention applies the sintering process commonly used for larger size to the micron-scale three-dimensional structure to realize metal filling and electrical interconnection, has smaller requirements on the shape of the structure, especially the depth-to-width ratio, can be flexibly applied to the structure which can not be realized by electroplating, and improves the compatibility. The whole process is in a liquid-free environment, so that the influence of instability of liquid and generation of bubbles on the micron-scale structure is avoided to the maximum extent. In the selection of metal powders, powders of various compositions require a prealloying process due to the "Brazilian effect" (the upward movement of particles with large diameters) that can occur during the vibration process. And a repeated filling process of filling, vibrating, removing floating powder, filling and vibrating is adopted, SEM images of samples after the silicon substrate is removed after filling and sintering are shown in figures 10-15, and the filling effect is good. The sintering environment adopts a high proportion of inert gas to match with a certain concentration of reducing gas, and the product is prevented from being oxidized. In addition, the clamp is designed into a double-layer matching mode of an upper-layer through groove structure, so that the demolding difficulty is reduced, and the yield is effectively improved. Meanwhile, the process is simple, compared with the traditional electroplating process, the time is greatly shortened, the efficiency is improved, and the method is suitable for batch production and improves the productivity.
This embodiment integrates high aspect ratio via structures and surface level structures, and filling can be accomplished using both electroplating and sintering. The invention is suitable for all similar structures, and has greater advantages on three-dimensional complex high-aspect-ratio structures, so the method is used for the example.
The above-mentioned embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solution of the present invention by those skilled in the art should fall within the protection scope defined by the claims of the present invention without departing from the spirit of the present invention.
Claims (10)
1. A three-dimensional MEMS structure metal filling method based on powder sintering is characterized in that metal powder is used for filling a three-dimensional MEMS structure and then sintering is carried out in a protective gas atmosphere.
2. The powder sintering based three-dimensional MEMS structure metal filling method of claim 1, characterized in that the metal powder is pre-alloyed powder of copper-tin alloy, copper-aluminum alloy or copper-zinc alloy.
3. The powder sintering based three-dimensional MEMS structure metal filling method of claim 2, wherein the copper-tin alloy prealloyed powder has a copper-tin volume ratio of 1:1, average particle size 15 μm.
4. The powder sintering based three-dimensional MEMS structure metal filling method of claim 1, wherein the protective gas is an inert gas.
5. The powder sintering based three-dimensional MEMS structure metal filling method of claim 4, wherein the inert gas is nitrogen or argon.
6. The powder sintering-based metal filling method for the three-dimensional MEMS structure according to claim 5, wherein the concentration of the nitrogen is 90-100%.
7. The powder sintering based three-dimensional MEMS structure metal filling method of claim 4, wherein the shielding gas further comprises a reducing gas.
8. The powder sintering based three-dimensional MEMS structure metal filling method of claim 6, wherein the reducing gas is hydrogen or carbon monoxide.
9. The powder sintering based three-dimensional MEMS structure metal filling method of claim 8, wherein the hydrogen gas concentration is below 10%.
10. The metal filling method for the three-dimensional MEMS structure based on powder sintering according to any one of claims 1 to 9, characterized by comprising the following steps:
firstly, pre-laying metal powder in a fixture with an upper through groove;
step (2) placing the test piece on the powder;
pouring metal powder into the clamp through the through groove until the metal powder covers the test piece, and placing the test piece on a vibration table for vibration;
removing powder on the upper surface after fully vibrating;
repeating the pouring and vibrating steps for 2-3 times;
step (6), placing the clamp filled with the metal powder and the test piece in a high-temperature annealing furnace, and sintering in a protective gas atmosphere;
step (7), completing sintering, and separating the clamp;
and (8) taking out a sample, and thinning and polishing to obtain the complete three-dimensional MEMS structure.
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Inventor after: Xu Tiantong Inventor after: Li Haiwang Inventor after: Zhai Yanxin Inventor after: Tao Zhi Inventor after: Huang Yujia Inventor after: Sun Jiamian Inventor before: Xu Tiantong Inventor before: Li Haiwang Inventor before: Tao Zhi Inventor before: Huang Yujia Inventor before: Sun Jiamian Inventor before: Zhai Yanxin |