CN117088704A - Integrated connection method of SiC-based composite material and application of SiC-based composite material in preparation of semiconductor SiC vacuum chuck - Google Patents
Integrated connection method of SiC-based composite material and application of SiC-based composite material in preparation of semiconductor SiC vacuum chuck Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 95
- 239000004065 semiconductor Substances 0.000 title claims abstract description 72
- 238000002360 preparation method Methods 0.000 title claims abstract description 53
- 239000002131 composite material Substances 0.000 title claims abstract description 21
- 229910004339 Ti-Si Inorganic materials 0.000 claims abstract description 123
- 229910010978 Ti—Si Inorganic materials 0.000 claims abstract description 123
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 96
- 239000000956 alloy Substances 0.000 claims abstract description 96
- 239000000843 powder Substances 0.000 claims abstract description 49
- 238000005245 sintering Methods 0.000 claims abstract description 28
- 230000008595 infiltration Effects 0.000 claims abstract description 26
- 238000001764 infiltration Methods 0.000 claims abstract description 26
- 238000011065 in-situ storage Methods 0.000 claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 238000003892 spreading Methods 0.000 claims abstract description 4
- 230000007480 spreading Effects 0.000 claims abstract description 4
- 239000002245 particle Substances 0.000 claims description 118
- 239000006229 carbon black Substances 0.000 claims description 35
- 239000011856 silicon-based particle Substances 0.000 claims description 28
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 26
- 239000000498 cooling water Substances 0.000 claims description 26
- 229910052802 copper Inorganic materials 0.000 claims description 26
- 239000010949 copper Substances 0.000 claims description 26
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 23
- 239000005011 phenolic resin Substances 0.000 claims description 23
- 229920001568 phenolic resin Polymers 0.000 claims description 23
- 238000005304 joining Methods 0.000 claims description 22
- 238000003825 pressing Methods 0.000 claims description 21
- 238000002844 melting Methods 0.000 claims description 19
- 230000008018 melting Effects 0.000 claims description 19
- 239000011148 porous material Substances 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 14
- 238000003466 welding Methods 0.000 claims description 13
- 238000005469 granulation Methods 0.000 claims description 12
- 230000003179 granulation Effects 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 11
- 238000000465 moulding Methods 0.000 claims description 8
- 239000011230 binding agent Substances 0.000 claims description 7
- 238000000498 ball milling Methods 0.000 claims description 6
- 238000009694 cold isostatic pressing Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 230000005496 eutectics Effects 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 3
- 238000007514 turning Methods 0.000 claims description 3
- 238000004364 calculation method Methods 0.000 claims description 2
- 239000013078 crystal Substances 0.000 claims description 2
- 230000002572 peristaltic effect Effects 0.000 claims description 2
- 239000007921 spray Substances 0.000 claims description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 166
- 229910010271 silicon carbide Inorganic materials 0.000 description 164
- 238000005516 engineering process Methods 0.000 description 70
- 238000010438 heat treatment Methods 0.000 description 33
- 239000011812 mixed powder Substances 0.000 description 31
- 239000000463 material Substances 0.000 description 30
- 238000005219 brazing Methods 0.000 description 24
- 239000002994 raw material Substances 0.000 description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 20
- 230000000052 comparative effect Effects 0.000 description 18
- 230000008569 process Effects 0.000 description 18
- 238000010008 shearing Methods 0.000 description 18
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- 238000003723 Smelting Methods 0.000 description 12
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- 239000002002 slurry Substances 0.000 description 11
- 239000002904 solvent Substances 0.000 description 11
- 238000000889 atomisation Methods 0.000 description 10
- 235000015895 biscuits Nutrition 0.000 description 9
- 239000000919 ceramic Substances 0.000 description 9
- 229910000676 Si alloy Inorganic materials 0.000 description 5
- 229910010293 ceramic material Inorganic materials 0.000 description 5
- 238000011068 loading method Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
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- 239000002184 metal Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 229910000679 solder Inorganic materials 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000001476 alcoholic effect Effects 0.000 description 2
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Classifications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
- C04B2237/30—Composition of layers of ceramic laminates or of ceramic or metallic articles to be joined by heating, e.g. Si substrates
- C04B2237/40—Metallic
Abstract
The invention relates to an integrated connection method of a SiC-based composite material and application of the integrated connection method in preparation of a semiconductor SiC vacuum chuck. The integrated connection method of the SiC-based composite material comprises the following steps: spreading Ti-Si alloy powder onto at least two SiC/C porous prefabricated blanks stacked, and performing in-situ reaction infiltration sintering to realize the integrated connection of the SiC-based composite material.
Description
Technical Field
The invention relates to an integrated connection technology applied to a semiconductor SiC vacuum chuck, in particular to an integrated connection method of a SiC-based composite material and application of the SiC-based composite material in preparing the semiconductor SiC vacuum chuck, and more particularly relates to a semiconductor SiC vacuum chuck which is compact and has certain connection strength by combining an in-situ infiltration method and a brazing connection technology through infiltration treatment of porous preforms by Ti-Si alloy particles by taking SiC powder, si particles, ti particles and carbon black as raw materials, belonging to the field of semiconductor material connection.
Background
As an important high-temperature structural material, silicon carbide (SiC) ceramic has the characteristics of small atomic radius, long bond length, strong covalent bond and the like, so that the silicon carbide (SiC) ceramic has the remarkable advantages of excellent high-temperature mechanical property, wear resistance, chemical corrosion resistance, high oxidation resistance temperature, small thermal expansion coefficient, radiation resistance and the like, and is widely applied to the fields of high precision tips such as precision machining, petrochemistry, transportation, aerospace, nuclear energy and the like. In addition, siC also has the functional characteristics of high heat conductivity, large forbidden bandwidth, high critical breakdown electric field, large electron saturation drift rate and the like, so that the SiC is widely applied to high-temperature, high-frequency, high-power and radiation-resistant semiconductor components and is recognized as a third-generation wide forbidden bandwidth semiconductor material with great development prospect. The active elements such as Ti, ta, cr, zr, V and the like are introduced into the SiC ceramic to prepare the SiC-based composite material, so that the regulation and control on the chemical property and the mechanical property of the SiC-based ceramic can be realized, and meanwhile, the higher conductivity and the oxidation resistance are kept, so that the SiC-based composite material has a good application prospect. In addition, siC has the disadvantages of high brittleness, poor workability, etc., making the manufacture of large-sized and complex-shaped parts challenging. At present, the connection technology of SiC ceramic materials is developed rapidly, and mainly comprises the following categories: direct connection, metal braze connection, solid diffusion bonding, precursor connection, MAX connection, and the like.
In these above-described connection schemes, there are mainly the following disadvantages:
1) Coefficient of thermal expansion mismatch: ceramic materials generally have a low coefficient of thermal expansion, and are subject to thermal stress and cracking when temperature changes due to a large difference from other materials such as metals. Friability and friability;
2) The ceramic material has brittleness and fragility, is easy to crack and damage, and limits the connection strength and reliability;
3) Difficult processing: ceramic materials generally have high hardness and high melting point, have high processing difficulty and require special processes and equipment;
4) Connection strength limit: ceramic materials generally have lower bond strengths than metallic materials and are prone to failure and breakage.
Therefore, a new connection mode applicable to SiC ceramics is required to be searched. Brazing is one of the most widely used methods in ceramic connection, has a good engineering application background, and in the brazing connection process, the welding stress caused by mismatch of thermal expansion coefficients between a ceramic base metal and a metal solder is always one of the technical difficulties which plague the silicon carbide ceramic brazing.
Disclosure of Invention
Aiming at the defects of the existing preparation and connection technology of the semiconductor SiC vacuum chuck, the invention provides an integrated connection technology for preparing the semiconductor SiC vacuum chuck which is compact and has certain connection strength by combining an in-situ infiltration method and a brazing connection technology for the first time.
Specifically, the invention provides an integrated connection method of a SiC-based composite material, which comprises the following steps: the Ti-Si alloy particles are spread on a SiC/C porous prefabricated blank body which is formed by stacking two or more blocks, and the SiC-based composite material is prepared and integrally connected through in-situ reaction infiltration sintering.
In the invention, the Ti-Si eutectic solder and the SiC base material have good chemical compatibility, and the thermal expansion coefficient of the Ti-Si eutectic solder is close to that of the SiC ceramic, so that the stress of a welded joint is reduced.
In the invention, porous preformed body is infiltrated by Ti-Si alloy particles, and the in-situ infiltration method and the brazing connection technology are combined to prepare the compact semiconductor SiC vacuum chuck with certain connection strength. The preparation and the integrated connection technology of SiC are completed in one step, the two-step process of brazing connection after sintering preparation is not needed, and the method is convenient and simple in process, low in cost, high in efficiency and good in industrial application prospect. The connection technology has important significance in the field of semiconductor material connection, and has non-abradable pushing effect on the progress of the semiconductor industrial production technology and the improvement of the production efficiency. Through searching, no patent and paper report of the in-situ reaction synthesis technology exists at present.
According to the invention, the SiC preparation and the integrated connection technology are completed in one step, the two-step process of brazing connection after sintering preparation is not needed, the process is convenient and simple, the cost is low, the efficiency is high, and the method has a good industrial application prospect. The connection technology has important significance in the field of semiconductor material connection, and has non-abradable pushing effect on the progress of the semiconductor industrial production technology and the improvement of the production efficiency.
Preferably, the mass fraction of Ti in the Ti-Si alloy powder is 25-45 wt.%; the grain size of the Ti-Si alloy powder is 3-5 mm. The invention can regulate and control the relative performance of the prepared SiC with certain connection strength by regulating and controlling the content of Ti in the Ti-Si alloy and the C of the initial raw material component, namely SiC.
Preferably, the preparation process of the Ti-Si alloy powder comprises the following steps:
(1) Mixing Ti particles and Si particles in proportion, placing the mixture in a water-cooled copper crucible, and cooling the mixture to room temperature after vacuum arc melting to obtain an ingot;
(2) Repeating the step (1) for 5-7 times, and turning over the prepared cast ingot for 180 degrees each time to obtain a Ti-Si co-crystal ingot;
(3) And crushing the obtained Ti-Si eutectic ingot to obtain Ti-Si alloy particles.
Preferably, the grain diameter of the Ti particles is 3-5 mm, and the purity is more than or equal to 99.9%; the grain diameter of the Si particles is 3-5 mm, and the purity is more than or equal to 99.9%;
The parameters of the vacuum arc melting include: vacuum degree is less than or equal to 8 multiplied by 10 -3 Pa; the current range is 120-260A; the temperature of the cooling water used for the water-cooled copper crucible is 22-24 ℃, and the pressure of the cooling water is 0.1-0.2 MPa.
Preferably, the pore diameter of each SiC/C porous preform body is 400 nm-1.5 mu m, the porosity is 3.63-8.13%, and the thickness is 1-10 mm, preferably 3-6 mm;
the SiC/C porous preform body comprises SiC powder and carbon black, wherein the mass ratio of the SiC powder to the carbon black is 1: (0.1-0.66);
the preparation process of the SiC/C porous prefabricated blank comprises the following steps: and mixing SiC powder, carbon black and a binder through ball milling, atomizing, granulating and forming to obtain the SiC/C porous prefabricated blank.
Preferably, the particle size of the SiC powder is 5-50 mu m, and the purity is more than or equal to 99.9%; the particle size of the carbon black is 1-5 mu m, and the purity is more than or equal to 99.9%;
the binder is at least one of phenolic resin, PVB and PVA, and is preferably phenolic resin; the mass fraction of the binder is 6-10 wt.% of the total mass of the SiC powder and the carbon black. The binder used herein was a 50wt.% phenolic resin alcoholic solution.
Preferably, the ball milling mixing parameters include: the rotating speed is 300-400 r/min, and the time is 240-300 min; the parameters of the spray granulation include: peristaltic speed is 30-60 r/min; the temperature is 90-100 ℃;
The molding mode comprises dry press molding and cold isostatic pressing molding; the pressure of the dry pressing molding is 4-6 MPa, and the time is 30-60S; the pressure of the cold isostatic pressing is 180-200 MPa, and the time is 10-15 min.
Preferably, the in-situ reaction infiltration sintering comprises: the atmosphere is vacuum or inert atmosphere; the temperature is 1400-1500 ℃; the heat preservation time is 60-120 min;
wherein the spreading amount of the Ti-Si alloy particles is 1.5 to 2.0 times of the theoretical calculation value.
Preferably, the in-situ reaction infiltration sintering comprises: at less than or equal to 5 multiplied by 10 -3 Under the vacuum condition of Pa, the temperature is increased to 1100-1200 ℃ at 8-12 ℃/min, then to 1200-1300 ℃ at 3-7 ℃/min, then to 1400-1500 ℃ at 1-3 ℃/min, the welding temperature is increased to 1400-1500 ℃, the temperature is kept for 60-120 min, and then the furnace is cooled to the room temperature.
On the other hand, the invention provides an application of an integrated connection method of a SiC-based composite material in preparing a semiconductor SiC vacuum chuck, wherein Ti-Si alloy powder is spread on at least two SiC/C porous prefabricated blanks which are stacked, and integrated connection of the SiC-based composite material is realized through in-situ reaction infiltration sintering; the SiC/C porous prefabricated blank is a semiconductor SiC vacuum chuck porous prefabricated blank;
The diameter of the porous prefabricated blank of the semiconductor SiC vacuum chuck is 100-350 mm;
the width of an air passage in the porous prefabricated blank of the semiconductor SiC vacuum chuck is 3-5 mm, and the depth is 2-4 mm;
the thickness of the porous prefabricated blank of the semiconductor SiC vacuum chuck is 3-10 mm, preferably 5-8 mm.
Preferably, the pore diameter of each SiC/C porous preform body is 400 nm-1.5 mu m, and the porosity is 3.63-8.13%; the SiC/C porous preform body comprises SiC powder and carbon black, wherein the mass ratio of the SiC powder to the carbon black is 1: (0.1-0.66).
The beneficial effects are that:
the porous preform is subjected to infiltration treatment through Ti-Si alloy particles, and the in-situ infiltration method and the brazing connection technology are combined to prepare the compact semiconductor SiC vacuum chuck with certain connection strength. The preparation and the integrated connection technology of SiC are completed in one step, the two-step process of brazing connection after sintering preparation is not needed, and the method is convenient and simple in process, low in cost, high in efficiency and good in industrial application prospect. The connection technology has important significance in the field of semiconductor material connection, and has non-abradable pushing effect on the progress of the semiconductor industrial production technology and the improvement of the production efficiency.
Drawings
FIG. 1 is a graph showing the microstructure of the Ti-Si alloy prepared in example 1, from which it is known that the Ti-Si alloy is successfully prepared by arc melting and the microstructure of the inside of the Ti-Si alloy is composed of rod-like TiSi 2 Eutectic colonies are uniformly distributed in the Si matrix;
FIG. 2 is a diagram showing the implementation of the reactive infiltration sintering process of SiC and a semiconductor SiC vacuum chuck prepared by connecting the integrated connection technology applied to the semiconductor SiC vacuum chuck in example 1;
FIG. 3 is a particle size distribution in a body of a SiC/C porous preform;
fig. 4 is a microscopic morphology diagram of the SiC-based composite connection interface prepared and connected by the integrated connection technique of example 1, and it can be seen from the figure that the composite connected by this method has uniform particle distribution and good contact interface, no pollution, no defect and higher bonding strength.
Detailed Description
The invention is further illustrated by the following embodiments, which are to be understood as merely illustrative of the invention and not limiting thereof.
Aiming at the defects of the existing preparation and connection technology of the semiconductor SiC vacuum chuck, the invention provides an integrated connection technology for preparing the semiconductor SiC vacuum chuck which is compact and has certain connection strength by combining an in-situ infiltration method and a brazing connection technology for the first time.
The following exemplifies an integrated connection technique applied to a semiconductor SiC vacuum chuck.
According to the Ti-Si binary phase diagram, ti particles and Si particles are weighed according to mass percent and mechanically mixed, are placed in a water-cooled copper crucible, are smelted for 5-7 times by adopting vacuum arc smelting equipment, are turned over for 180 degrees each time, and are naturally cooled to room temperature under the vacuum condition, so that the preparation of Ti-Si alloy powder is completed. The raw materials used for the Ti-Si alloy component comprise Si particles and Ti particles. The grain diameter of the Si particles is 3-5 mm, and the purity is more than or equal to 99.9%; the grain diameter of Ti particles is 3-5 mm, and the purity is more than or equal to 99.9%. Wherein the vacuum degree of the arc melting furnace is better than 8 multiplied by 10 -3 Pa, the current range is 120-260A, the temperature of cooling water of the copper crucible is 22-24 ℃, and the pressure of the cooling water is 0.1-0.2 MPa. In addition, the Ti-Si alloy after arc melting is crushed into Ti-Si alloy particles with uniform particle size of 3-5 mm by using a vibration mill.
According to the invention, siC powder and carbon black are taken as raw materials, the SiC powder and the carbon black are weighed according to the mass percentage designed by each component, the proportioned powder is uniformly mixed, and the powder is pressed into a green body. The mixing method is not particularly limited, and ball milling may be used, and the ball milling solvent is 50wt.% phenolic resin alcoholic solution. The method adopted by the pressing is a dry pressing method, the mixed powder is filled into a mould with specified size, and a certain pressure (for example, 4-6 MPa) is applied to form the powder, so that a blank of the SiC/C porous preform is prepared.
The crushed Ti-Si alloy particles are placed on a green body of SiC/C porous prefabricated body which takes SiC powder and carbon black as raw materials, is uniformly mixed according to a certain proportion and is at least two stacked.
The compact SiC with certain connection strength is prepared by sintering the blank through an integrated connection technology combining an in-situ infiltration method and a brazing connection technology. Uniformly placing the uniformly crushed Ti-Si alloy particles on a blank of at least two SiC/C porous preforms stacked, wherein the placement theory needs Ti-Si alloy particles with the amount of 1.5-2 times that of the Ti-Si alloy particles, so as to ensure that the blank can be completely infiltrated.
Placing the blank in a vacuum brazing furnace to complete the vacuum brazing process, and realizing an integrated connection technology of SiC, wherein the connection technology comprises the following steps: at less than or equal to 5 multiplied by 10 -3 Under the vacuum condition of Pa, the temperature is increased to 1100-1200 ℃ at 8-12 ℃/min, then to 1200-1300 ℃ at 3-7 ℃/min, then to 1400-1500 ℃ at 1-3 ℃/min, the welding temperature is increased to 1400-1500 ℃, the temperature is kept for 60-120 min, and then the furnace is cooled to the room temperature.
In the invention, the integrated connection technology applied to the semiconductor SiC vacuum chuck is adopted, and the conductivity of the semiconductor SiC with certain connection strength prepared by the method is 1.74 multiplied by 10 -4 ～5.12×10 -5 S cm -1 Within the range.
In the invention, the integrated connection technology applied to the semiconductor SiC vacuum chuck is adopted, and the vacuum suction strength of the semiconductor SiC vacuum chuck connected by the method is 1.5 multiplied by 10 -10 ～1.1×10 -11 PaWm 3 ·S -1 。
The present invention will be further illustrated by the following examples. It is also to be understood that the following examples are given solely for the purpose of illustration and are not to be construed as limitations upon the scope of the invention, since numerous insubstantial modifications and variations will now occur to those skilled in the art in light of the foregoing disclosure. The specific process parameters and the like described below are also merely examples of suitable ranges, i.e., one skilled in the art can make a suitable selection from the description herein and are not intended to be limited to the specific values described below.
Example 1:
(1) Preparation of Ti-Si alloy: weighing Ti particles and Si particles according to a certain mass ratio according to a Ti-Si binary phase diagram and making the machineMechanical mixing, placing in a water-cooled copper crucible, smelting for 5-7 times by adopting vacuum arc smelting equipment, turning over an ingot for 180 degrees each time, and naturally cooling to room temperature under the vacuum condition to finish the preparation of the Ti-Si co-ingot. Wherein, the grain diameter of the Si particles is 3-5 mm, and the purity is more than or equal to 99.9%; the grain diameter of Ti particles is 3-5 mm, and the purity is more than or equal to 99.9%. The vacuum degree of the arc melting furnace is 5 multiplied by 10 -3 Pa, current 200A, cooling water temperature of the copper crucible 22 ℃, and cooling water pressure 0.15MPa. In addition, the Ti-Si alloy is pulverized into Ti-Si alloy grains having a uniform grain size of 3 to 5mm by using a vibration mill.
(2) Preparing a blank: (1) preparation of mixed powder: uniformly mixing SiC powder (particle size of 5 mu m, purity of more than or equal to 99.9%), carbon black (particle size of 1-5 mu m, purity of more than or equal to 99.9%) and 50wt.% phenolic resin with ethanol as a solvent by using a planetary ball mill, and atomizing the prepared slurry into mixed powder with uniform size through atomization and granulation; (2) pressing a blank: the mixed powder obtained in the step (1) is filled into a rectangular mold with the thickness of 36.00 multiplied by 52.00mm, and the pressure of 4-6MPa is applied to prepare a rectangular tabletting sample with the thickness of 36.00 multiplied by 52.00mm, so as to prepare the SiC/C porous preform body. Wherein the pore size distribution of the preform is 400 nm-1.0 mu m, the porosity is 3.63%, and the thickness is 5.0mm.
The raw materials and proportions used in example 1 are shown in Table 1:
| name of the name | Particle size | Proportioning (wt.) |
| Ti | 3～5mm | 25.00 |
| Si | 3～5mm | 75.00 |
| SiC | 5μm | 83.42 |
| Carbon black | 1～5μm | 8.58 |
| Phenolic resin | - | 8.00 |
。
(3) An integrated connection technology: the Ti-Si alloy particles with uniform size prepared in the step (1) are laid on the blank with two SiC/C porous prefabricated bodies which are stacked and placed in the step (2), and the Ti-Si alloy particles which are 1.5 to 2 times of the theoretical Ti-Si alloy particles are placed, so that the blank can be completely infiltrated, the placed biscuit is placed in a vacuum brazing furnace, and an integrated connection technology is carried out, wherein the connection technology comprises the following steps: at less than or equal to 5 multiplied by 10 -3 Heating to 1200 ℃ at 10 ℃/min, heating to 1300 ℃ at 5 ℃/min, heating to 1500 ℃ at 2 ℃/min, welding at the temperature of 1500 ℃ at the vacuum condition of Pa, preserving heat for 120min, and cooling to room temperature along with a furnace.
In this example 1, the particle size distribution in the body of the SiC/C porous preform was as shown in FIG. 3A, the particle size was mainly concentrated around 0.67 μm and 5.92. Mu.m, and the dispersion was uniform. In addition, the microscopic morphology diagram of the connection interface of the semiconductor SiC which is prepared by the integrated connection technology and is compact and has certain connection strength is shown in fig. 4, and the graph shows that the interface of the SiC material which is connected by the integrated connection technology has good bonding, no pollution and no defect and has higher bonding strength. This is achieved by an integrated connection technique applied to a semiconductor SiC vacuum chuckThe shearing strength of the SiC material prepared by the method reaches 56MPa, and the conductivity is 3.75X10 -4 S cm -1 。
Example 2:
(1) Preparation of Ti-Si alloy: according to a Ti-Si binary phase diagram, ti particles and Si particles are weighed according to a certain mass ratio and mechanically mixed, placed in a water-cooled copper crucible, smelted for 5-7 times by adopting vacuum arc smelting equipment, the cast ingot is turned over for 180 degrees each time, and naturally cooled to room temperature under a vacuum condition, so that the preparation of the Ti-Si co-ingot is completed. Wherein, the grain diameter of the Si particles is 3-5 mm, and the purity is more than or equal to 99.9%; the grain diameter of Ti particles is 3-5 mm, and the purity is more than or equal to 99.9%. The vacuum degree of the arc melting furnace is 8 multiplied by 10 -3 Pa, current 220A, cooling water temperature of the copper crucible 23 ℃, and cooling water pressure of 0.1MPa. In addition, the Ti-Si alloy is pulverized into Ti-Si alloy grains having a uniform grain size of 3 to 5mm by using a vibration mill.
(2) Preparing a blank: (1) preparation of mixed powder: uniformly mixing SiC powder (particle size of 10 mu m, purity of more than or equal to 99.9%), carbon black (particle size of 1-5 mu m, purity of more than or equal to 99.9%) and 50wt.% of phenolic resin by using ethanol as a solvent and using a planetary ball mill, and atomizing the prepared slurry into mixed powder with uniform size through atomization and granulation; (2) pressing a blank: the mixed powder obtained in the step (1) is filled into a rectangular mold with the thickness of 36.00 multiplied by 52.00mm, and the pressure of 4-6MPa is applied to prepare a rectangular tabletting sample with the thickness of 36.00 multiplied by 52.00mm, so as to prepare the SiC/C porous preform body. Wherein the pore size distribution of the preform is 600 nm-1.2 mu m, the porosity is 4.63%, and the thickness is 5.0mm.
The raw materials and proportions used in this example 2 are shown in Table 2:
| name of the name | Particle size | Proportioning (wt.) |
| Ti | 3～5mm | 25.00 |
| Si | 3～5mm | 75.00 |
| SiC | 10μm | 83.42 |
| Carbon black | 1～5μm | 8.58 |
| Phenolic resin | - | 8.00 |
。
(3) An integrated connection technology: the Ti-Si alloy particles with uniform size prepared in the step (1) are laid on the blank with two SiC/C porous prefabricated bodies which are stacked and placed in the step (2), and the Ti-Si alloy particles which are 1.5 to 2 times of the theoretical Ti-Si alloy particles are placed, so that the blank can be completely infiltrated, the placed biscuit is placed in a vacuum brazing furnace, and an integrated connection technology is carried out, wherein the connection technology comprises the following steps: at less than or equal to 5 multiplied by 10 -3 Heating to 1200 ℃ at 10 ℃/min, heating to 1300 ℃ at 5 ℃/min, heating to 1500 ℃ at 2 ℃/min, welding at the temperature of 1500 ℃ at the vacuum condition of Pa, preserving heat for 120min, and cooling to room temperature along with a furnace.
In this example 2, the particle size distribution in the body of the SiC/C porous preform was as shown in FIG. 3B, the particle size was mainly concentrated around 0.67 μm and 9.86. Mu.m, and the dispersion was uniform. Through an integral body applied to semiconductor SiC vacuum chuckChemical connection technology the shearing strength of the SiC material prepared by the method reaches 63MPa, and the conductivity is 1.25 multiplied by 10 -4 S cm -1 。
Example 3
(1) Preparation of Ti-Si alloy: according to a Ti-Si binary phase diagram, ti particles and Si particles are weighed according to a certain mass ratio and mechanically mixed, placed in a water-cooled copper crucible, smelted for 5-7 times by adopting vacuum arc smelting equipment, the cast ingot is turned over for 180 degrees each time, and naturally cooled to room temperature under a vacuum condition, so that the preparation of the Ti-Si co-ingot is completed. Wherein, the grain diameter of the Si particles is 3-5 mm, and the purity is more than or equal to 99.9%; the grain diameter of Ti particles is 3-5 mm, and the purity is more than or equal to 99.9%. The vacuum degree of the arc melting furnace is 2 multiplied by 10 -3 Pa, current 180A, cooling water temperature of the copper crucible 22 ℃, and cooling water pressure of 0.2MPa. In addition, the Ti-Si alloy is pulverized into Ti-Si alloy grains having a uniform grain size of 3 to 5mm by using a vibration mill.
(2) Preparing a blank: (1) preparation of mixed powder: uniformly mixing SiC powder (particle size of 10 mu m, purity of more than or equal to 99.9%), carbon black (particle size of 1-5 mu m, purity of more than or equal to 99.9%) and 50wt.% of phenolic resin by using ethanol as a solvent and using a planetary ball mill, and atomizing the prepared slurry into mixed powder with uniform size through atomization and granulation; (2) pressing a blank: the mixed powder obtained in the step (1) is filled into a rectangular mold with the thickness of 36.00 multiplied by 52.00mm, and the pressure of 4-6MPa is applied to prepare a rectangular tabletting sample with the thickness of 36.00 multiplied by 52.00mm, so as to prepare the SiC/C porous preform body. Wherein the pore size distribution of the preform is 900 nm-1.5 mu m, the porosity is 8.13%, and the thickness is 5.0mm.
The raw materials and proportions used in this example 3 are shown in Table 3:
| name of the name | Particle size | Proportioning (wt.) |
| Ti | 3～5mm | 25.00 |
| Si | 3～5mm | 75.00 |
| SiC | 50μm | 83.42 |
| Carbon black | 1～5μm | 8.58 |
| Phenolic resin | - | 8.00 |
。
(3) An integrated connection technology: the Ti-Si alloy particles with uniform size prepared in the step (1) are laid on the blank with two SiC/C porous prefabricated bodies which are stacked and placed in the step (2), and the Ti-Si alloy particles which are 1.5 to 2 times of the theoretical Ti-Si alloy particles are placed, so that the blank can be completely infiltrated, the placed biscuit is placed in a vacuum brazing furnace, and an integrated connection technology is carried out, wherein the connection technology comprises the following steps: at less than or equal to 5 multiplied by 10 -3 Heating to 1200 ℃ at 10 ℃/min, heating to 1300 ℃ at 5 ℃/min, heating to 1500 ℃ at 2 ℃/min, welding at the temperature of 1500 ℃ at the vacuum condition of Pa, preserving heat for 120min, and cooling to room temperature along with a furnace.
In this example 3, the particle size distribution in the body of the SiC/C porous preform was as shown in FIG. 3C, and the particle size was mainly concentrated around 0.49 μm, 1.45 μm and 12.76. Mu.m, and the dispersion was relatively uniform. By an application to semiconductorsSiC material prepared by the method has shearing strength of 49MPa and conductivity of 4.25 multiplied by 10 -4 S cm -1 。
Example 4
(1) Preparation of Ti-Si alloy: according to a Ti-Si binary phase diagram, ti particles and Si particles are weighed according to a certain mass ratio and mechanically mixed, placed in a water-cooled copper crucible, smelted for 5-7 times by adopting vacuum arc smelting equipment, the cast ingot is turned over for 180 degrees each time, and naturally cooled to room temperature under a vacuum condition, so that the preparation of the Ti-Si co-ingot is completed. Wherein, the grain diameter of the Si particles is 3-5 mm, and the purity is more than or equal to 99.9%; the grain diameter of Ti particles is 3-5 mm, and the purity is more than or equal to 99.9%. The vacuum degree of the arc melting furnace is 3 multiplied by 10 -3 Pa, current 230A, cooling water temperature of the copper crucible 23 ℃, and cooling water pressure of 0.2MPa. In addition, the Ti-Si alloy is pulverized into Ti-Si alloy grains having a uniform grain size of 3 to 5mm by using a vibration mill.
(2) Preparing a blank: (1) preparation of mixed powder: siC powder (particle size 5-50 μm, purity not less than 99.9%, carbon black (particle size 1-5 μm, purity not less than 99.9%), three kinds of powder and 50wt.% phenolic resin are uniformly mixed by using an epicyclic ball mill with ethanol as a solvent, and the prepared slurry is atomized into mixed powder with uniform size through atomization and granulation, (2) pressing a blank, namely loading the mixed powder obtained in step (1) into a rectangular mold with 36.00 multiplied by 52.00mm, applying pressure of 4-6MPa, preparing a rectangular tabletting sample with 36.00 multiplied by 52.00mm, and preparing a SiC/C porous preform body, wherein the pore size distribution of the preform body is 400 nm-1.1 μm, the porosity is 4.23%, and the thickness is 6.0mm.
The raw materials and proportions used in this example 4 are shown in Table 4:
(3) An integrated connection technology: laying the Ti-Si alloy particles with uniform size prepared in the step (1) on the surface2) The prepared blank with two SiC/C porous prefabricated bodies stacked is placed on the blank, ti-Si alloy particles which are 1.5-2 times of the theoretical required Ti-Si alloy particles are placed, the blank body can be completely infiltrated, the placed blank is placed in a vacuum brazing furnace, and an integrated connection technology is carried out, wherein the connection technology comprises the following steps: at less than or equal to 5 multiplied by 10 -3 Heating to 1200 ℃ at 10 ℃/min, heating to 1300 ℃ at 5 ℃/min, heating to 1450 ℃ at 2 ℃/min, welding at the temperature of 1450 ℃ at vacuum condition of Pa, preserving heat for 120min, and cooling to room temperature along with a furnace.
In example 4, the dense semiconductor SiC interface prepared by the integrated joining technique and having a certain joining strength was well bonded, free of contamination, free of defects, and had a higher bonding strength. In addition, the shearing strength of the SiC material prepared by the method reaches 59MPa, and the conductivity is 4.17 multiplied by 10 -5 S cm -1 。
Example 5
(1) Preparation of Ti-Si alloy: according to a Ti-Si binary phase diagram, ti particles and Si particles are weighed according to a certain mass ratio and mechanically mixed, placed in a water-cooled copper crucible, smelted for 5-7 times by adopting vacuum arc smelting equipment, the cast ingot is turned over for 180 degrees each time, and naturally cooled to room temperature under a vacuum condition, so that the preparation of the Ti-Si co-ingot is completed. Wherein, the grain diameter of the Si particles is 3-5 mm, and the purity is more than or equal to 99.9%; the grain diameter of Ti particles is 3-5 mm, and the purity is more than or equal to 99.9%. The vacuum degree of the arc melting furnace is 8 multiplied by 10 -3 Pa, current 160A, cooling water temperature of the copper crucible 23 ℃, and cooling water pressure of 0.15MPa. In addition, the Ti-Si alloy is pulverized into Ti-Si alloy grains having a uniform grain size of 3 to 5mm by using a vibration mill.
(2) Preparing a blank: (1) preparation of mixed powder: siC powder (particle size 5-50 mu m, purity not less than 99.9%, carbon black (particle size 1-5 mu m, purity not less than 99.9%), three kinds of powder and 50wt.% phenolic resin are uniformly mixed by using an epicyclic ball mill with ethanol as a solvent, and the prepared slurry is atomized into mixed powder with uniform size through atomization and granulation, (2) pressing a blank, namely loading the mixed powder obtained in step (1) into a rectangular mold with 36.00 multiplied by 52.00mm, applying pressure of 4-6MPa, preparing a rectangular tabletting sample with 36.00 multiplied by 52.00mm, and preparing a SiC/C porous prefabricated blank, wherein the pore size distribution of the prefabricated blank is 500 nm-1.0 mu m, the porosity is 3.97%, and the thickness is 7.0mm.
The raw materials and proportions used in this example 5 are shown in Table 5:
(3) An integrated connection technology: the Ti-Si alloy particles with uniform size prepared in the step (1) are laid on the blank with two SiC/C porous prefabricated bodies which are stacked and placed in the step (2), and the Ti-Si alloy particles which are 1.5 to 2 times of the theoretical Ti-Si alloy particles are placed, so that the blank can be completely infiltrated, the placed biscuit is placed in a vacuum brazing furnace, and an integrated connection technology is carried out, wherein the connection technology comprises the following steps: at less than or equal to 5 multiplied by 10 -3 Heating to 1200 ℃ at 10 ℃/min, heating to 1300 ℃ at 5 ℃/min, heating to 1500 ℃ at 2 ℃/min, welding at the temperature of 1500 ℃ at the vacuum condition of Pa, preserving heat for 90min, and cooling to room temperature along with a furnace.
In example 5, the dense semiconductor SiC interface prepared by the integrated joining technique and having a certain joining strength was well bonded, free of contamination, free of defects, and had a higher bonding strength. In addition, the shearing strength of the SiC material prepared by the method reaches 61MPa, and the conductivity is 8.15X10 -4 S cm -1 。
Example 6
(1) Preparation of Ti-Si alloy: according to a Ti-Si binary phase diagram, ti particles and Si particles are weighed according to a certain mass ratio and mechanically mixed, placed in a water-cooled copper crucible, smelted for 5-7 times by adopting vacuum arc smelting equipment, the cast ingot is turned over for 180 degrees each time, and naturally cooled to room temperature under a vacuum condition, so that the preparation of the Ti-Si co-ingot is completed. Wherein, the grain diameter of the Si particles is 3-5 mm, and the purity is more than or equal to 99.9%; the grain diameter of Ti particles is 3-5 mm, and the purity is more than or equal to 99.9%. The vacuum degree of the arc melting furnace is 4 multiplied by 10 -3 Pa, current 250A, copper crucibleThe cooling water temperature is 23 ℃, and the cooling water pressure is 0.15MPa. In addition, the Ti-Si alloy is pulverized into Ti-Si alloy grains having a uniform grain size of 3 to 5mm by using a vibration mill.
(2) Preparing a blank: (1) preparation of mixed powder: siC powder (particle size 10 μm, purity not less than 99.9%, carbon black (particle size 1-5 μm, purity not less than 99.9%), three kinds of powder and 50wt.% phenolic resin are uniformly mixed by using a planetary ball mill with ethanol as a solvent, and the prepared slurry is atomized into mixed powder with uniform size through atomization and granulation, (2) pressing a blank, namely placing the mixed powder obtained in step (1) into a rectangular mold with 36.00 multiplied by 52.00mm, applying pressure of 4-6MPa, and preparing a rectangular tabletting sample with 36.00 multiplied by 52.00mm, and preparing a SiC/C porous preform, wherein the pore size distribution of the preform is 600 nm-1.1 μm, the porosity is 4.56%, and the thickness is 8.0mm.
The raw materials and proportions used in this example 6 are shown in Table 6:
(3) An integrated connection technology: the Ti-Si alloy particles with uniform size, which are prepared in the step (1), are laid on the blank of the SiC/C porous preform, which is prepared in the step (2) and is stacked, and Ti-Si alloy particles, which are 1.5 to 2 times of the theoretical Ti-Si alloy particles, are placed, so that the blank can be completely infiltrated, the placed biscuit is placed in a vacuum brazing furnace, and an integrated connection technology is carried out, wherein the connection technology comprises the following steps: at less than or equal to 5 multiplied by 10 -3 Heating to 1200 ℃ at 10 ℃/min, heating to 1300 ℃ at 5 ℃/min, heating to 1400 ℃ at 2 ℃/min, welding at the temperature of 1400 ℃, preserving heat for 120min, and cooling to room temperature along with a furnace.
In example 5, the dense semiconductor SiC interface prepared by the integrated joining technique and having a certain joining strength was well bonded, free of contamination, free of defects, and had a higher bonding strength. In addition, by this methodThe shearing strength of the prepared SiC material reaches 60MPa, and the conductivity is 2.75X10 -5 S cm -1 。
Example 7
(1) Preparation of Ti-Si alloy: according to a Ti-Si binary phase diagram, ti particles and Si particles are weighed according to a certain mass ratio and mechanically mixed, placed in a water-cooled copper crucible, smelted for 5-7 times by adopting vacuum arc smelting equipment, the cast ingot is turned over for 180 degrees each time, and naturally cooled to room temperature under a vacuum condition, so that the preparation of the Ti-Si co-ingot is completed. Wherein, the grain diameter of the Si particles is 3-5 mm, and the purity is more than or equal to 99.9%; the grain diameter of Ti particles is 3-5 mm, and the purity is more than or equal to 99.9%. The vacuum degree of the arc melting furnace is 5 multiplied by 10 -3 Pa, current 260A, cooling water temperature of the copper crucible 24 ℃, and cooling water pressure of 0.1MPa. In addition, the Ti-Si alloy is pulverized into Ti-Si alloy grains having a uniform grain size of 3 to 5mm by using a vibration mill.
(2) Preparing a blank: (1) preparation of mixed powder: siC powder (particle size 10 μm, purity not less than 99.9%, carbon black (particle size 1-5 μm, purity not less than 99.9%), three kinds of powder and 50wt.% phenolic resin are uniformly mixed by using a planetary ball mill with ethanol as a solvent, and the prepared slurry is atomized into mixed powder with uniform size through atomization and granulation, (2) pressing of a blank, namely loading the mixed powder obtained in step (1) into a rectangular mold with 36.00 multiplied by 52.00mm, and applying pressure of 4-6MPa to prepare a rectangular tabletting sample with 36.00 multiplied by 52.00mm, so as to prepare a SiC/C porous preform, wherein the pore size distribution of the preform is 500 nm-1.2 μm, the porosity is 6.97%, and the thickness is 5.0mm.
The raw materials and proportions used in this example 7 are shown in Table 7:
(3) An integrated connection technology: laying the Ti-Si alloy particles with uniform size prepared in the step (1) on the SiC/C porous prefabricated body prepared in the step (2) and placed by two blocks in a stacking wayThe Ti-Si alloy particles which are 1.5 to 2 times of the theoretical required Ti-Si alloy particles are placed, the blank body can be completely infiltrated, the placed biscuit is placed into a vacuum brazing furnace for an integrated connection technology, and the connection technology comprises the following steps: at less than or equal to 5 multiplied by 10 -3 Heating to 1200 ℃ at 10 ℃/min, heating to 1300 ℃ at 5 ℃/min, heating to 1450 ℃ at 2 ℃/min under the vacuum condition of Pa, preserving heat for 90min, and cooling to room temperature along with a furnace.
In example 6, the dense semiconductor SiC interface prepared by the integrated joining technique and having a certain joining strength was well bonded, free of contamination, free of defects, and had a higher bonding strength. In addition, the shearing strength of the SiC material prepared by the method reaches 62MPa, and the conductivity is 9.25X10 -4 S cm -1 。
Example 8
(1) Preparation of Ti-Si alloy: according to a Ti-Si binary phase diagram, ti particles and Si particles are weighed according to a certain mass ratio and mechanically mixed, placed in a water-cooled copper crucible, smelted for 5-7 times by adopting vacuum arc smelting equipment, the cast ingot is turned over for 180 degrees each time, and naturally cooled to room temperature under a vacuum condition, so that the preparation of the Ti-Si co-ingot is completed. Wherein, the grain diameter of the Si particles is 3-5 mm, and the purity is more than or equal to 99.9%; the grain diameter of Ti particles is 3-5 mm, and the purity is more than or equal to 99.9%. The vacuum degree of the arc melting furnace is 3 multiplied by 10 -3 Pa, current 170A, cooling water temperature of the copper crucible 23 ℃, and cooling water pressure of 0.2MPa. In addition, the Ti-Si alloy is pulverized into Ti-Si alloy grains having a uniform grain size of 3 to 5mm by using a vibration mill.
(2) Preparing a blank: (1) preparation of mixed powder: siC powder (particle size 10 μm, purity not less than 99.9%, carbon black (particle size 1-5 μm, purity not less than 99.9%), three kinds of powder and 50wt.% phenolic resin are uniformly mixed by using a planetary ball mill with ethanol as a solvent, and the prepared slurry is atomized into mixed powder with uniform size through atomization and granulation, (2) pressing a blank, namely placing the mixed powder obtained in step (1) into a rectangular mold with 36.00 multiplied by 52.00mm, applying pressure of 4-6MPa, and preparing a rectangular tabletting sample with 36.00 multiplied by 52.00mm, and preparing a SiC/C porous preform, wherein the pore size distribution of the preform is 400-1.0 μm, the porosity is 3.96%, and the thickness is 6.0mm.
The raw materials and proportions used in this example 8 are shown in Table 8:
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(3) An integrated connection technology: the Ti-Si alloy particles with uniform size, which are prepared in the step (1), are laid on the blank of the SiC/C porous preform, which is prepared in the step (2) and is stacked, and Ti-Si alloy particles, which are 1.5 to 2 times of the theoretical Ti-Si alloy particles, are placed, so that the blank can be completely infiltrated, the placed biscuit is placed in a vacuum brazing furnace, and an integrated connection technology is carried out, wherein the connection technology comprises the following steps: at less than or equal to 5 multiplied by 10 -3 Heating to 1200 ℃ at 10 ℃/min, heating to 1300 ℃ at 5 ℃/min, heating to 1400 ℃ at 2 ℃/min, welding at the temperature of 1400 ℃ at the vacuum condition of Pa, preserving heat for 90min, and cooling to room temperature along with a furnace.
In example 5, the dense semiconductor SiC interface prepared by the integrated joining technique and having a certain joining strength was well bonded, free of contamination, free of defects, and had a higher bonding strength. In addition, the shearing strength of the SiC material prepared by the method reaches 61MPa, and the conductivity is 6.45 multiplied by 10 -4 S cm -1 。
Example 9
(1) Preparation of Ti-Si alloy: according to a Ti-Si binary phase diagram, ti particles and Si particles are weighed according to a certain mass ratio and mechanically mixed, placed in a water-cooled copper crucible, smelted for 5-7 times by adopting vacuum arc smelting equipment, the cast ingot is turned over for 180 degrees each time, and naturally cooled to room temperature under a vacuum condition, so that the preparation of the Ti-Si co-ingot is completed. Wherein, the grain diameter of the Si particles is 3-5 mm, and the purity is more than or equal to 99.9%; the grain diameter of Ti particles is 3-5 mm, and the purity is more than or equal to 99.9%. The vacuum degree of the arc melting furnace is 6 multiplied by 10 -3 Pa, current 240A, cooling water temperature of the copper crucible 24 ℃, and cooling water pressure of 0.2MPa. In addition, use is made ofThe Ti-Si alloy is crushed into Ti-Si alloy particles with uniform particle size, and the particle size is 3-5 mm by a vibration mill.
(2) Preparing a blank: (1) preparation of mixed powder: siC powder (particle size 10 μm, purity not less than 99.9%, carbon black (particle size 1-5 μm, purity not less than 99.9%), three kinds of powder and 50wt.% phenolic resin are uniformly mixed by using a planetary ball mill with ethanol as a solvent, and the prepared slurry is atomized into mixed powder with uniform size through atomization and granulation, (2) pressing a blank, namely placing the mixed powder obtained in step (1) into a rectangular mold with 36.00 multiplied by 52.00mm, applying pressure of 4-6MPa, and preparing a rectangular tabletting sample with 36.00 multiplied by 52.00mm, and preparing a SiC/C porous preform, wherein the pore size distribution of the preform is 800 nm-1.3 μm, the porosity is 6.63%, and the thickness is 7.0mm.
The raw materials and proportions used in this example 9 are shown in Table 9:
(3) An integrated connection technology: the Ti-Si alloy particles with uniform size, which are prepared in the step (1), are laid on the blank of the SiC/C porous preform, which is prepared in the step (2) and is stacked, and Ti-Si alloy particles, which are 1.5 to 2 times of the theoretical Ti-Si alloy particles, are placed, so that the blank can be completely infiltrated, the placed biscuit is placed in a vacuum brazing furnace, and an integrated connection technology is carried out, wherein the connection technology comprises the following steps: at less than or equal to 5 multiplied by 10 -3 Heating to 1200 ℃ at 10 ℃/min, heating to 1300 ℃ at 5 ℃/min, heating to 1400 ℃ at 2 ℃/min, welding at the temperature of 1400 ℃, preserving heat for 120min, and cooling to room temperature along with a furnace.
In example 9, the dense semiconductor SiC interface prepared by the integrated joining technique and having a certain joining strength was well bonded, free of contamination, free of defects, and had a higher bonding strength. In addition, the shearing strength of the SiC material prepared by the method reaches 55MPa, and the conductivity is 2.51X10 -4 S cm -1 。
Example 10
(1) Preparation of Ti-Si alloy: according to a Ti-Si binary phase diagram, ti particles and Si particles are weighed according to a certain mass ratio and mechanically mixed, placed in a water-cooled copper crucible, smelted for 5-7 times by adopting vacuum arc smelting equipment, the cast ingot is turned over for 180 degrees each time, and naturally cooled to room temperature under a vacuum condition, so that the preparation of the Ti-Si co-ingot is completed. Wherein, the grain diameter of the Si particles is 3-5 mm, and the purity is more than or equal to 99.9%; the grain diameter of Ti particles is 3-5 mm, and the purity is more than or equal to 99.9%. The vacuum degree of the arc melting furnace is 7 multiplied by 10 -3 Pa, current 210A, cooling water temperature of the copper crucible 23 ℃, and cooling water pressure of 0.15MPa. In addition, the Ti-Si alloy is pulverized into Ti-Si alloy grains having a uniform grain size of 3 to 5mm by using a vibration mill.
(2) Preparing a blank: (1) preparation of mixed powder: siC powder (particle size 10 μm, purity not less than 99.9%, carbon black (particle size 1-5 μm, purity not less than 99.9%), three kinds of powder and 50wt.% phenolic resin are uniformly mixed by using a planetary ball mill with ethanol as a solvent, and the prepared slurry is atomized into mixed powder with uniform size through atomization and granulation, (2) pressing of a blank, namely loading the mixed powder obtained in step (1) into a rectangular mold with 36.00 multiplied by 52.00mm, and applying pressure of 4-6MPa to prepare a rectangular tabletting sample with 36.00 multiplied by 52.00mm, so as to prepare a SiC/C porous preform, wherein the pore size distribution of the preform is 700 nm-1.2 μm, the porosity is 7.63%, and the thickness is 9.0mm.
The raw materials and proportions used in this example 10 are shown in Table 10:
(3) An integrated connection technology: laying the Ti-Si alloy particles with uniform size, which are prepared in the step (1), on the blank of the SiC/C porous prefabricated body, which is prepared in the step (2) and is placed in a stacking way, wherein the theoretical requirement of the placement of the Ti-Si alloy particles is 1.5The Ti-Si alloy particles which are about 2 times of the size can be completely infiltrated, the placed biscuit is placed into a vacuum brazing furnace for an integrated connection technology, and the connection technology comprises the following steps: at less than or equal to 5 multiplied by 10 -3 Heating to 1200 ℃ at 10 ℃/min, heating to 1300 ℃ at 5 ℃/min, heating to 1500 ℃ at 2 ℃/min, welding at the temperature of 1500 ℃ at the vacuum condition of Pa, preserving heat for 90min, and cooling to room temperature along with a furnace.
In example 10, the dense semiconductor SiC interface with a certain bonding strength prepared by the integrated bonding technique was well bonded, free of contamination, defect free, and had a high bonding strength. In addition, the shearing strength of the SiC material prepared by the method reaches 53MPa, and the conductivity is 7.25X10 -4 S cm -1 。
Example 11
This embodiment 11 is different from the specific embodiment 1 in that: in the reaction infiltration sintering of the step (3), the sintering temperature is 1400 ℃, and the temperature is kept for 120min, and the other steps are the same as those of the specific example 1. The semiconductor SiC of example 11, which was dense and has a certain bonding strength, produced by the integrated bonding technique, had good interfacial bonding, was free of contamination, was defect-free, and had a high bonding strength. The shearing strength of the SiC material prepared by the method reaches 54MPa and the conductivity is 8.75X10 by an integrated connection technology applied to a semiconductor SiC vacuum chuck -4 S cm -1 。
Example 12
This embodiment 12 is different from the specific embodiment 1 in that: in the reaction infiltration sintering of the step (3), the sintering temperature is 1400 ℃, and the temperature is kept for 90 minutes, and the other steps are the same as those of the specific example 1. The semiconductor SiC of example 12, which is dense and has a certain bonding strength, has good interfacial bonding, no contamination, no defects, and a high bonding strength. The shearing strength of the SiC material prepared by the method reaches 48MPa and the conductivity is 1.75X10 by an integrated connection technology applied to a semiconductor SiC vacuum chuck -5 S cm -1 。
Example 13
This embodiment 13 is different from the specific embodiment 1 in that: step (3) reverseIn the infiltration sintering, the sintering temperature is 14400 ℃, and the temperature is kept for 60 minutes, otherwise, the same as in the specific example 1 is adopted. The semiconductor SiC of example 13, which was dense and has a certain bonding strength, produced by the integrated bonding technique, had good interfacial bonding, was free of contamination, was defect-free, and had a high bonding strength. The shearing strength of the SiC material prepared by the method reaches 45MPa and the conductivity is 1.22 multiplied by 10 by an integrated connection technology applied to a semiconductor SiC vacuum chuck -5 S cm -1 。
Example 14
This embodiment 14 is different from the specific embodiment 1 in that: in the preparation of the Ti-Si alloy in the step (1), the Ti content in the Ti-Si alloy is different, the raw material ratio is shown in Table 11, and the other materials are the same as those in the embodiment 1.
The raw materials and proportions used in example 14 are shown in Table 11:
| name of the name | Particle size | Proportioning (wt.) |
| Ti | 3～5mm | 30.00 |
| Si | 3～5mm | 70.00 |
| SiC | 5μm | 83.42 |
| Carbon black | 1～5μm | 8.58 |
| Phenolic resin | - | 8.00 |
。
The semiconductor SiC of example 13, which was dense and has a certain bonding strength, produced by the integrated bonding technique, had good interfacial bonding, was free of contamination, was defect-free, and had a high bonding strength. The shearing strength of the SiC material prepared by the method reaches 52MPa and the conductivity is 7.22 multiplied by 10 by an integrated connection technology applied to a semiconductor SiC vacuum chuck -4 S cm -1 。
Example 15
This example 15 differs from the specific example 1 in that: in the preparation of the Ti-Si alloy in the step (1), the Ti content in the Ti-Si alloy is different, the raw material ratio is shown in Table 12, and the other steps are the same as those in the embodiment 1.
The raw materials and proportions used in example 14 are shown in Table 12:
| name of the name | Particle size | Proportioning (wt.) |
| Ti | 3～5mm | 35.00 |
| Si | 3～5mm | 65.00 |
| SiC | 5μm | 83.42 |
| Carbon black | 1～5μm | 8.58 |
| Phenolic resin | - | 8.00 |
。
The dense semiconductor SiC prepared by the integrated joining technique in example 15, which has a certain joining strength, has good interfacial bonding, is free of contamination and defects, and has a high joining strength. The shearing strength of the SiC material prepared by the method reaches 55MPa and the conductivity is 3.25 multiplied by 10 by an integrated connection technology applied to a semiconductor SiC vacuum chuck -4 S cm -1 。
Example 16
This embodiment 16 is different from the specific embodiment 1 in that: in the preparation of the blank in the step (2), the SiC is changed from the C of the SiC/C porous prefabricated blank, the raw material ratio is shown in Table 13, and the other materials are the same as those in the embodiment 1.
The raw materials and proportions used in example 16 are shown in Table 13:
| name of the name | Particle size | Proportioning (wt.) |
| Ti | 3～5mm | 25.00 |
| Si | 3～5mm | 75.00 |
| SiC | 5μm | 82.50 |
| Carbon black | 1～5μm | 9.50 |
| Phenolic resin | - | 8.00 |
。
The semiconductor SiC of example 16, which is dense and has a certain bonding strength, has good interfacial bonding, no contamination, no defects, and a high bonding strength. The shearing strength of the SiC material prepared by the method reaches 53MPa and the conductivity is 7.25 multiplied by 10 by an integrated connection technology applied to a semiconductor SiC vacuum chuck -4 S cm -1 。
Example 17
This embodiment 16 is different from the specific embodiment 1 in that: in the preparation of the blank in the step (2), the SiC is changed from the C of the SiC/C porous prefabricated blank, the raw material ratio is shown in Table 14, and the other materials are the same as those in the embodiment 1.
The raw materials and proportions used in example 17 are shown in Table 14:
| name of the name | Particle size | Proportioning (wt.) |
| Ti | 3～5mm | 25.00 |
| Si | 3～5mm | 75.00 |
| SiC | 5μm | 73.50 |
| Carbon black | 1～5μm | 18.50 |
| Phenolic resin | - | 8.00 |
。
The semiconductor SiC of example 17, which was dense and has a certain bonding strength, produced by the integrated bonding technique, had good interfacial bonding, was free of contamination, was defect-free, and had a high bonding strength. Such a connection technique is integrated by an integrated connection technique applied to a semiconductor SiC vacuum chuckThe shearing strength of the SiC material prepared by the method reaches 51MPa, and the conductivity is 9.17 multiplied by 10 -4 S cm -1 。
Example 18
This embodiment 18 is different from the specific embodiment 1 in that: in the preparation of the body of step (2), the SiC/C porous preform body was in the shape of a semiconductor vacuum suction disc (diameter 250mm, width of air passage 3mm, depth 3mm, thickness 10 mm), and its specific illustration was the same as that of example 1, except that it was shown in fig. 2. The dense semiconductor SiC vacuum chuck with a certain bonding strength prepared by the integrated bonding technique in this example 18 has good interface bonding, no contamination, no defect, and higher bonding strength. The shearing strength of the SiC material prepared by the method reaches 56MPa and the conductivity is 3.75X10 by an integrated connection technology applied to a semiconductor SiC vacuum chuck -4 S cm -1 Vacuum suction strength was 6.5X10 - 10 Pa·m 3 ·S -1 。
Comparative example 1
This comparative example 1 differs from the specific example 1 in that: in the preparation of the blank in the step (2), a pressure of 4-6MPa is applied to prepare a 36.00 multiplied by 52.00mm rectangular tabletting sample, and the sample is subjected to cold isostatic pressing (200 MPa, and pressure maintaining is carried out for 15 min) to prepare a SiC/C porous prefabricated blank, otherwise the same as in the specific example 1. The semiconductor SiC of comparative example 1, which is dense and has a certain bonding strength, cannot be prepared by the integrated bonding technique, because the internal pores thereof are changed after cold isostatic pressing, thereby making the ti—si alloy particles impermeable to the porous preform.
Comparative example 2
This comparative example 2 differs from the specific example 1 in that: in the step (3) integrated joining technique, the placed green compact was placed in a vacuum sintering furnace (vacuum degree 5 to 30 Pa) and sintered in the same manner as in example 1. The semiconductor SiC of this comparative example 1 cannot be prepared to be dense and have a certain connection strength by the integrated connection technique because connection cannot be performed during infiltration of ti—si alloy particles due to a low degree of vacuum during sintering.
Comparative example 3
This comparative example 3 differs from the specific example 1 in that: in the step (3) integrated connection technology, the heating rate is not changed, a one-step heating rate method is implemented, and the specific sintering process is as follows: at less than or equal to 5 multiplied by 10 -3 Heating to 1400 ℃ at 10 ℃/min under Pa vacuum condition, maintaining the temperature for 120min, and cooling to room temperature along with the furnace, wherein the other steps are the same as those of the embodiment 1. The semiconductor SiC of comparative example 3 cannot be produced to be dense and have a certain connection strength by the integral connection technique because the sintering rate is too fast during sintering, it cannot be completely performed during the reaction, and thus the inside thereof cannot be penetrated, and "sandwiches" occur and accompanies the process of being unable to connect.
Comparative example 4
This comparative example 4 differs from the specific example 1 in that: this comparative example 4 differs from the specific example 1 in that: in the step (3) integrated joining technique, a slurry coating process of a layer of ti—si alloy was performed before stacking and placing, otherwise the same as in embodiment 1. In this comparative example 4, a dense semiconductor SiC having a certain connection strength cannot be prepared by the integrated connection technique, because the coating of the slurry claims a reaction layer on the surface of the green body during sintering, thereby preventing the further infiltration process of ti—si alloy particles, and making it impossible to realize a one-step connection process.
Comparative example 5
This comparative example 5 differs from the specific example 1 in that: two porous SiC/C preforms (20 mm) having a thickness four times the thickness (5 mm) of the porous SiC/C preform used in example 1 were stacked (total thickness 40 mm) and then subjected to in-situ infiltration sintering. In the comparative example 1, a dense semiconductor SiC with a certain connection strength cannot be prepared by an integrated connection technology, because the Ti-Si alloy cannot be completely infiltrated in the sintering infiltration process due to thicker samples, and thus the Ti-Si alloy particles are incompletely connected in the infiltration process and the matrix has a "clamping" phenomenon.
Table 15 shows the composition and melting parameters of Ti-Si alloys in the preparation steps of examples and comparative examples applied to the integrated connection technique of semiconductor SiC vacuum chucks:
table 16 shows the composition of the greenware and its integral connection parameters for the examples and comparative examples in an integral connection technique applied to a semiconductor SiC vacuum chuck:
the embodiments described above are possible embodiments of the present invention, but the embodiments of the present invention are not limited to the embodiments described above, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principle of the present invention should be made in the equivalent manner, and the embodiments are included in the protection scope of the present invention.
Claims (11)
1. An integrated connection method of a SiC-based composite material, comprising: spreading Ti-Si alloy powder onto at least two SiC/C porous prefabricated blanks stacked, and performing in-situ reaction infiltration sintering to realize the integrated connection of the SiC-based composite material.
2. The integrated connection method according to claim 1, wherein the mass fraction of Ti in the Ti-Si alloy powder is 25-45 wt.%; the grain size of the Ti-Si alloy powder is 3-5 mm.
3. The integrated joining method according to claim 2, wherein the Ti-Si alloy powder is prepared by the steps of:
(1) Mixing Ti particles and Si particles in proportion, placing the mixture in a water-cooled copper crucible, and cooling the mixture to room temperature after vacuum arc melting to obtain an ingot;
(2) Repeating the step (1) for 5-7 times, and turning over the prepared cast ingot for 180 degrees each time to obtain a Ti-Si co-crystal ingot;
(3) And crushing the obtained Ti-Si eutectic ingot to obtain Ti-Si alloy particles.
4. The integrated connection method according to claim 3, wherein the grain diameter of the Ti particles is 3-5 mm, and the purity is more than or equal to 99.9%; the grain diameter of the Si particles is 3-5 mm, and the purity is more than or equal to 99.9%;
the parameters of the vacuum arc melting include: vacuum degree is less than or equal to 8 multiplied by 10 -3 Pa; the current range is 120-260A; the temperature of the cooling water used for the water-cooled copper crucible is 22-24 ℃, and the pressure of the cooling water is 0.1-0.2 MPa.
5. The integrated joining method according to any one of claims 1 to 4, characterized in that each SiC/C porous preform has a pore size of 400nm to 1.5 μm, a porosity of 3.63 to 8.13% and a thickness of 1 to 10mm, preferably 3 to 6mm;
the SiC/C porous preform body comprises SiC powder and carbon black, wherein the mass ratio of the SiC powder to the carbon black is 1: (0.1-0.66);
the preparation process of the SiC/C porous prefabricated blank comprises the following steps: and mixing SiC powder, carbon black and a binder through ball milling, atomizing, granulating and forming to obtain the SiC/C porous prefabricated blank.
6. The integrated connection method according to claim 5, wherein the particle size of the SiC powder is 5 to 50 μm, and the purity is not less than 99.9%; the particle size of the carbon black is 1-5 mu m, and the purity is more than or equal to 99.9%;
the binder is at least one of phenolic resin, PVB and PVA, and is preferably phenolic resin; the mass fraction of the binder is 6-10 wt.% of the total mass of the SiC powder and the carbon black.
7. The integrated joining method according to claim 5, wherein the parameters of the ball-milling mixing include: the rotating speed is 300-400 r/min, and the time is 240-300 min;
The parameters of the spray granulation include: peristaltic speed is 30-60 r/min; the temperature is 90-100 ℃;
the molding mode comprises dry press molding and cold isostatic pressing molding; the pressure of the dry pressing molding is 4-6 MPa, and the time is 30-60S; the pressure of the cold isostatic pressing is 180-200 MPa, and the time is 10-15 min.
8. The integrated joining method according to any one of claims 1 to 4, wherein the in situ reactive infiltration sintering comprises: the atmosphere is vacuum or inert atmosphere; the temperature is 1400-1500 ℃; the heat preservation time is 60-120 min;
wherein the spreading amount of the Ti-Si alloy particles is 1.5 to 2.0 times of the theoretical calculation value.
9. The integrated joining method according to claim 8, wherein the in situ reactive infiltration sintering comprises: at less than or equal to 5 multiplied by 10 -3 Under the vacuum condition of Pa, the temperature is raised to 1100-1200 ℃ at 8-12 ℃/min, then raised to 1200-1300 ℃ at 3-7 ℃/min, then raised to the welding temperature of 1400-1500 ℃ at 1-3 ℃/min, and the furnace is cooled to the room temperature after heat preservation for 60-120 min.
10. Use of an integrated connection method of a SiC-based composite material according to any one of claims 1 to 9 for the preparation of a semiconductor SiC vacuum chuck, characterized in that Ti-Si alloy powder is spread onto at least two stacked SiC/C porous preform bodies, and integrated connection of the SiC-based composite material is achieved by in-situ reactive infiltration sintering; the SiC/C porous prefabricated blank is a semiconductor SiC vacuum chuck porous prefabricated blank;
The diameter of the porous prefabricated blank of the semiconductor SiC vacuum chuck is 100-350 mm;
the width of an air passage in the porous prefabricated blank of the semiconductor SiC vacuum chuck is 3-5 mm, and the depth is 2-4 mm;
the thickness of the porous prefabricated blank of the semiconductor SiC vacuum chuck is 3-10 mm.
11. Use according to claim 10, characterized in that the pore size of each SiC/C porous preform is 400 nm-1.5 μm and the porosity is 3.63-8.13%; the SiC/C porous preform body comprises SiC powder and carbon black, wherein the mass ratio of the SiC powder to the carbon black is 1: (0.1-0.66).
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| CN116813358A (en) * | 2023-06-21 | 2023-09-29 | 杭州沈氏节能科技股份有限公司 | Forming process of silicon carbide plate and silicon carbide plate prepared by forming process |
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