CN115584212A - Silicon material adhesive and preparation method and use method thereof - Google Patents
Silicon material adhesive and preparation method and use method thereof Download PDFInfo
- Publication number
- CN115584212A CN115584212A CN202211322087.5A CN202211322087A CN115584212A CN 115584212 A CN115584212 A CN 115584212A CN 202211322087 A CN202211322087 A CN 202211322087A CN 115584212 A CN115584212 A CN 115584212A
- Authority
- CN
- China
- Prior art keywords
- adhesive
- glass powder
- expansion coefficient
- bonding
- silicon material
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000000853 adhesive Substances 0.000 title claims abstract description 73
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 72
- 239000002210 silicon-based material Substances 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title abstract description 9
- 239000011521 glass Substances 0.000 claims abstract description 66
- 239000000843 powder Substances 0.000 claims abstract description 62
- 239000002904 solvent Substances 0.000 claims abstract description 28
- 239000000463 material Substances 0.000 claims abstract description 27
- 239000002562 thickening agent Substances 0.000 claims abstract description 25
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical group O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 27
- 239000000243 solution Substances 0.000 claims description 19
- 238000002156 mixing Methods 0.000 claims description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 17
- 238000002844 melting Methods 0.000 claims description 16
- 230000008018 melting Effects 0.000 claims description 16
- 239000004354 Hydroxyethyl cellulose Substances 0.000 claims description 12
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 claims description 12
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 claims description 12
- 238000003466 welding Methods 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 11
- 239000007864 aqueous solution Substances 0.000 claims description 9
- 239000000377 silicon dioxide Substances 0.000 claims description 7
- 238000005303 weighing Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 239000007767 bonding agent Substances 0.000 claims description 5
- 239000011248 coating agent Substances 0.000 claims description 3
- 238000000576 coating method Methods 0.000 claims description 3
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 2
- 239000013464 silicone adhesive Substances 0.000 claims description 2
- 229920001296 polysiloxane Polymers 0.000 claims 5
- 229910052710 silicon Inorganic materials 0.000 abstract description 12
- 239000010703 silicon Substances 0.000 abstract description 12
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 10
- 229910021420 polycrystalline silicon Inorganic materials 0.000 abstract description 10
- 239000000758 substrate Substances 0.000 abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 10
- 235000012239 silicon dioxide Nutrition 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- 230000035882 stress Effects 0.000 description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- 239000011259 mixed solution Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000005336 cracking Methods 0.000 description 3
- 239000003607 modifier Substances 0.000 description 3
- 239000010453 quartz Substances 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 235000012431 wafers Nutrition 0.000 description 3
- 239000001856 Ethyl cellulose Substances 0.000 description 2
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 229920001249 ethyl cellulose Polymers 0.000 description 2
- 235000019325 ethyl cellulose Nutrition 0.000 description 2
- 230000003301 hydrolyzing effect Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000013081 microcrystal Substances 0.000 description 2
- 239000006060 molten glass Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 229920005591 polysilicon Polymers 0.000 description 2
- 235000019353 potassium silicate Nutrition 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 230000003749 cleanliness Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910001867 inorganic solvent Inorganic materials 0.000 description 1
- 239000003049 inorganic solvent Substances 0.000 description 1
- 238000004518 low pressure chemical vapour deposition Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000000935 solvent evaporation Methods 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- 238000000427 thin-film deposition Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J1/00—Adhesives based on inorganic constituents
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Glass Compositions (AREA)
Abstract
The invention provides a silicon material adhesive and a preparation method and a using method thereof, wherein the silicon material adhesive comprises glass powder, an expansion coefficient regulator, a thickening agent and a solvent, and the mass ratio of the glass powder to the expansion coefficient regulator to the thickening agent is 30-50. The silicon material adhesive disclosed by the invention selects glass powder as an adhesive base material, is matched with an expansion coefficient regulator, is mixed in a specific proportion and dissolved in a solvent to form the adhesive with certain initial bonding strength, the glass powder is sintered and melted at high temperature to form firm and excellent-tightness bonding with a silicon substrate, and the expansion coefficient of the adhesive material is adjusted by the expansion coefficient regulator to enable the expansion coefficient of the adhesive material to be close to that of polycrystalline silicon, so that the internal stress of a bonding surface is reduced.
Description
Technical Field
The invention relates to the technical field of adhesives, in particular to a silicon material adhesive and a preparation method and a use method thereof.
Background
In a semiconductor polycrystalline silicon thin film deposition process (CVD-poly), an air guide pipe is needed to convey external process gas into a pipe cavity, and the air guide pipe needs to be heat-resistant and have enough cleanliness due to a high-temperature environment in the pipe cavity, so that quartz pipes are mostly used in the current 8-inch and 12-inch chip manufacturing process, but the quartz pipes have large difference between expansion coefficients and polycrystalline silicon, and need to face the problem of frequent equipment maintenance.
With the technical development of semiconductor silicon materials, the application scenes of the semiconductor silicon materials are more and more extensive, wherein the silicon materials can also be used for manufacturing gas guide tubes of CVD process equipment to replace quartz tubes. Because the air duct has great draw ratio, and the inlet section is the elbow structure, is difficult to accomplish an organic whole processing, and the air duct of silicon material needs to carry out machining. The prior art generally divides the pipe body into two male and female parts which are symmetrical along the axis, and the pipe body structure is formed by bonding, but the difference between the expansion coefficient of the existing bonding material and pure silicon is large, and huge internal stress can be brought by the bonding surface which penetrates through the whole pipe body.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide an adhesive for a silicon material airway so as to reduce the internal stress of an adhesive surface and avoid the airway from cracking.
In order to achieve the above object, a first aspect of the present invention provides a silica material adhesive, including glass powder, a coefficient of expansion modifier, a thickener, and a solvent, where a mass ratio of the glass powder to the coefficient of expansion modifier to the thickener is 30 to 50.
The silicon material adhesive disclosed by the invention selects glass powder as an adhesive base material, is matched with an expansion coefficient regulator, is mixed in a specific proportion and dissolved in a solvent to form the adhesive with certain initial bonding strength, the glass powder is sintered and melted at high temperature to form firm and excellent-tightness bonding with a silicon substrate, and the expansion coefficient of the adhesive material is adjusted by the expansion coefficient regulator to enable the expansion coefficient of the adhesive material to be close to that of polycrystalline silicon, so that the internal stress of a bonding surface is reduced.
Preferably, the glass frit has a onset temperature greater than 750 ℃. Because the working condition temperature of the wafer LPCVD process is less than 700 ℃, the initial melting temperature of the glass powder is limited, and the bonding material is solid under the working condition.
Preferably, the melting point of the glass powder is 850-900 ℃. The glass powder has a low melting point, is sintered and melted at a high temperature, and can form firm adhesion with a silicon substrate and excellent sealing property.
Preferably, the purity of the glass powder is more than 99.9 percent, and SiO in the glass powder 2 The content of (A) is more than 80%. The glass powder has high purity and is SiO 2 The content of the glass powder is high, so that the expansion coefficient of the glass powder is similar to that of polycrystalline silicon.
Preferably, the mesh number of the glass powder is more than 1500 meshes. The mesh number of the glass powder is limited so as to ensure that the powder cannot be settled too fast when being mixed into the solvent and ensure that the mixture is uniform.
Preferably, the expansion coefficient modifier is a silica sol solution.
Preferably, the expansion coefficient regulator contains silica sol with particle size less than 50nm and 20-40% of silica sol. The surface of the silicon dioxide sol has a large amount of silicon hydroxyl groups, and silicon dioxide microcrystal particles can be formed after hydrolytic condensation, so that a good particle state can be kept under a welding working condition all the time, glass powder melted at high temperature is well supported, the viscosity of liquid glass is increased, the glass is prevented from flowing and overflowing after being melted, and meanwhile, the overlarge dragging stress of the molten glass on a base material in the process of cooling and vitrifying can be reduced.
Preferably, the thickener is an aqueous solution of hydroxyethyl cellulose. Ethyl cellulose provides initial bond strength to the mixed adhesive after solvent evaporation.
The second aspect of the present invention provides a method for preparing the above silicon material adhesive, including the steps of: the method comprises the following steps: adding a thickening agent into a solvent, and uniformly mixing; weighing glass powder according to the mass requirement, adding the glass powder into a solvent with a thickening agent, and uniformly mixing; and adding an expansion coefficient regulator into the solution added with the thickening agent and the glass powder, and uniformly mixing.
The preparation method has the advantages that the thickening agent, the glass powder and the expansion coefficient regulator are dissolved in the solvent, the operation steps are simple, the field preparation is convenient, the quality and the stability of the adhesive are ensured, the adding sequence of the raw materials in the solvent is limited, and the raw materials can be uniformly mixed.
The third aspect of the present invention provides a method for using the above silicon material adhesive, including the steps of: coating the adhesive on the bonding surface of the silicon material part to be bonded; bonding the bonding surfaces of the silicon material parts to be bonded, and forming preliminary bonding after the solvent of the bonding agent is volatilized; putting the silicon material part into a high-temperature furnace for welding, wherein the welding temperature is 950-1100 ℃, and the adhesive is sintered and melted in the welding process to form adhesion with the silicon material; the bonding surface of the silicon material part after cooling has an expansion coefficient of 2.3-2.7 multiplied by 10 -6 Bonding material per deg.C.
The method comprises the steps of preliminarily bonding silicon material parts to be bonded, sintering and melting the bonding material at high temperature to form firm bonding with the silicon substrate and excellent in sealing property, wherein the expansion coefficient of the bonding material is close to that of polycrystalline silicon after cooling, so that the internal stress of a bonding surface is reduced, and when the bonding agent is used for bonding the silicon material gas guide tube, the tube body can be prevented from cracking, and the service life of the gas guide tube is prolonged.
Drawings
FIG. 1 is a schematic flow chart of a method for preparing a silicone adhesive according to an embodiment of the present invention;
fig. 2 is a flow chart illustrating a method for using a silicon adhesive according to an embodiment of the present invention.
Description of the drawings:
1-glass powder, 2-expansion coefficient regulator, 3-thickening agent, 4-solvent, 5-silicon material part and 6-high temperature furnace.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below. It should be noted that the following examples are only used to illustrate the implementation method and typical parameters of the present invention, and are not used to limit the scope of the parameters of the present invention, so that reasonable variations can be made and still fall within the protection scope of the claims of the present invention.
It is noted that the endpoints of the ranges and any values disclosed herein are not limited to the precise range or value and that such ranges or values are understood to encompass values close to such ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
The specific embodiment of the invention discloses a silicon material adhesive which is mainly used for bonding silicon material parts used by CVD process equipment and is particularly suitable for preparing silicon material gas-guide tubes. The silicon material adhesive comprises glass powder, an expansion coefficient regulator, a thickening agent and a solvent, wherein the mass ratio of the glass powder to the expansion coefficient regulator to the thickening agent is controlled to be 30-50.
The glass powder used by the adhesive has a low melting point and high purity, the purity is more than 99.9 percent, and SiO in the glass powder 2 The content of the glass powder is more than 80 percent, and the expansion coefficient of the glass powder is similar to that of the polysilicon. The initial melting temperature of the glass powder is more than 750 ℃, and the bonding material is solid under the working condition. The melting point of the glass powder is controlled to be 850-900 ℃, and the glass powder can be sintered and melted at high temperature. The mesh number of the glass powder is more than 1500 meshes, so that the powder cannot be precipitated too fast when mixed into a solvent.
The expansion coefficient regulator used for the adhesive is a silica sol solution, the particle size of the silica sol is less than 50nm, and the content of the silica sol is 20-40%. The surface of the silicon dioxide sol has a large amount of silicon hydroxyl groups, and silicon dioxide microcrystal particles can be formed after hydrolytic condensation, so that a good particle state can be kept under a welding working condition all the time, glass powder melted at high temperature is well supported, the viscosity of liquid glass is increased, the glass is prevented from flowing and overflowing after being melted, and meanwhile, the overlarge dragging stress of the molten glass on a base material in the process of cooling and vitrifying can be reduced.
The thickening agent used by the adhesive is hydroxyethyl cellulose aqueous solution, and ethyl cellulose provides initial adhesive strength of the mixed adhesive material after the solvent is volatilized.
The solvent used by the adhesive is an inorganic solvent, such as water, methanol, ethanol, acetone and the like, so that the glass powder, the expansion coefficient regulator and the thickening agent can be uniformly mixed in the solvent, a temporary stable state is kept, and the solvent can be quickly volatilized after the adhesive is coated.
The silicon material adhesive selects glass powder as an adhesive base material, is matched with an expansion coefficient regulator, is mixed in a specific proportion, is dissolved in a solvent to form the adhesive with certain initial bonding strength, and is sintered and melted at high temperature to form firm bonding with the silicon substrate and excellent sealing property.
As shown in fig. 1, the preparation method of the silicon material adhesive comprises the following steps:
s11, dropwise adding a thickening agent 3 into a solvent 4, and uniformly mixing;
s12, weighing the glass powder 1 according to the quality requirement, adding the glass powder into a solvent 4 with a thickening agent 3, and uniformly mixing;
s13, adding the expansion coefficient regulator 2 dropwise into the solvent 4 added with the thickening agent 3 and the glass powder 1, and mixing uniformly.
According to the preparation method, the thickening agent 3, the glass powder 1 and the expansion coefficient regulator 2 are dissolved in the solvent 4, the operation steps are simple, the field preparation is convenient, the quality and the stability of the adhesive are ensured, the adding sequence of the raw materials in the solvent is limited, and the raw materials can be uniformly mixed.
The specific implementation mode of the invention also discloses a using method of the silicon material adhesive, which is shown in a combined figure 2 and comprises the following steps:
s21, coating the adhesive on the bonding surface of the silicon material part 5 to be bonded;
s22, adhering the bonding surfaces of the silicon material parts 5 to be bonded, and forming preliminary bonding after the solvent of the bonding agent is volatilized;
s23, the silicon material part 5 is placed into a high-temperature furnace 5 for welding, the welding temperature is 950-1100 ℃, and the adhesive is sintered and melted in the welding process to form adhesion with the silicon material.
The method firstly carries out preliminary bonding on silicon material parts to be bonded, then leads the bonding material to be sintered and melted at high temperature, andthe silicon substrates form a firm and well-sealed bond, and the coefficient of expansion of the bonding material after cooling is 2.3-2.7 x 10 -6 The temperature per DEG C is similar to that of polycrystalline silicon, so that the internal stress of the bonding surface is reduced. When the adhesive is used for bonding the silicon material air duct, the tube body can be prevented from cracking, and the service life of the air duct is prolonged.
The present invention will be further described with reference to the following specific examples.
Example 1
Dripping 0.05ml of hydroxyethyl cellulose aqueous solution into 100ml of water, and uniformly mixing; weighing 2g of glass powder, wherein the mesh number of the glass powder is more than 1500 meshes, the purity is more than 99.9 percent, the initial melting temperature is 770 ℃, the melting point is 875 ℃, adding the glass powder into an aqueous solution containing hydroxyethyl cellulose, and uniformly mixing; and then 0.04ml of silica sol solution is dripped into the mixed solution, the particle size of the silica sol in the silica sol solution is less than 50nm, the content of the silica sol is 30 percent, and the adhesive is obtained after uniform mixing.
Example 2
0.04ml of hydroxyethyl cellulose aqueous solution is dripped into 80ml of acetone and mixed evenly; weighing 1.5g of glass powder, wherein the mesh number of the glass powder is more than 1500 meshes, the purity is more than 99.9 percent, the initial melting temperature is 800 ℃, the melting point is 900 ℃, adding the glass powder into an acetone solution containing hydroxyethyl cellulose, and uniformly mixing; and then 0.06ml of silica sol solution is dripped into the mixed solution, the particle size of the silica sol in the silica sol solution is less than 50nm, the content of the silica sol is 20 percent, and the adhesive is obtained by uniformly mixing.
Example 3
0.1ml of hydroxyethyl cellulose aqueous solution is dripped into 120ml of ethanol and is uniformly mixed; weighing 3g of glass powder, wherein the mesh number of the glass powder is more than 1500 meshes, the purity is more than 99.9 percent, the initial melting temperature is 760 ℃, the melting point is 860 ℃, adding the glass powder into an ethanol solution with hydroxyethyl cellulose, and uniformly mixing; and then 0.1ml of silica sol solution is dripped into the mixed solution, the particle size of the silica sol in the silica sol solution is less than 50nm, the content of the silica sol is 40 percent, and the adhesive is obtained after uniform mixing.
Example 4
Dripping 0.08ml of hydroxyethyl cellulose aqueous solution into 60ml of ethanol, and uniformly mixing; weighing 2.5g of glass powder, wherein the mesh number of the glass powder is more than 1500 meshes, the purity is more than 99.9 percent, the initial melting temperature is 790 ℃, the melting point is 900 ℃, and the glass powder is added into an ethanol solution with hydroxyethyl cellulose and mixed uniformly; and then 0.05ml of silica sol solution is dripped into the mixed solution, the particle size of the silica sol in the silica sol solution is less than 50nm, the content of the silica sol is 35 percent, and the adhesive is obtained by uniformly mixing.
Comparative example 1
This comparative example was different from example 1 in that the silica sol solution was not added and the other process steps were the same to obtain an adhesive.
Comparative example 2
This comparative example was different from example 2 in that the aqueous solution of hydroxyethyl cellulose was not added and the procedure was the same as in the other method to obtain an adhesive.
The adhesives prepared in examples 1 to 4 and comparative examples 1 to 2 were subjected to performance tests, the contents and methods of which are as follows.
(1) Initial adhesion strength test: preliminarily bonding the two silicon wafers, and testing according to the GB/T7124-2008 standard;
(2) And (3) testing tensile shear strength: welding the two silicon wafers, and performing a tensile shear test on the sample by using a universal mechanical tester at the temperature of 500 ℃;
(3) And (3) testing the expansion coefficient: and testing the bonding material formed after the bonding agent is sintered by adopting a thermal expansion instrument.
The test results are shown in table 1 below.
TABLE 1 Performance index of the adhesive
| Test object | Initial adhesion strength (Mpa) | Tensile shear strength (Mpa) | Coefficient of expansion (10) -6 /℃) |
| Example 1 | 1.2 | 4.5 | 2.5 |
| Example 2 | 1.3 | 4.3 | 2.6 |
| Example 3 | 1.2 | 4.6 | 2.5 |
| Example 4 | 1.1 | 4.2 | 2.4 |
| Comparative example 1 | 0.9 | 2.3 | 4.1 |
| Comparative example 2 | 0.4 | 4.1 | 2.7 |
According to the performance test results of the adhesives, the initial adhesive strength of the adhesives of the examples 1-4 is obviously higher than that of the adhesive of the comparative example 2, and the thickening agent added in the system plays a role in increasing the initial adhesive strength; the tensile shear strength of the sintered adhesive in the examples 1-4 is obviously higher than that of the adhesive in the comparative example 1, and the silica sol solution in the system plays a role in increasing the adhesive strength; examples 1-4 the expansion coefficient after sintering of the adhesive was 2.3 to 2.7X 10 -6 between/deg.C, similar to that of polysilicon, and the expansion coefficient of the adhesive of comparative example 1 after sintering is 4.1X 10 -6 The difference between the temperature per DEG C and the temperature per DEG C is larger than that of polycrystalline silicon, so that the effect of adjusting the expansion coefficient can be achieved by adding the silicon dioxide sol solution in the system, and the thermal stress of the bonding surface of the silicon material part is reduced.
Although the present invention is disclosed above, the present invention is not limited thereto. Various changes and modifications may be effected therein by one skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (10)
1. The silicon material adhesive is characterized by comprising glass powder, an expansion coefficient regulator, a thickening agent and a solvent, wherein the mass ratio of the glass powder to the expansion coefficient regulator to the thickening agent is (30-50).
2. The silicone material adhesive of claim 1, wherein the glass frit has a onset temperature greater than 750 ℃.
3. The silicone material adhesive agent as claimed in claim 2, wherein the melting point of the glass frit is 850 to 900 ℃.
4. A silicon material adhesive as claimed in claim 3, wherein the glass powder purity is greater than 99.9%, and the glass powder contains SiO 2 The content of (A) is more than 80%.
5. A silica material adhesive according to claim 4, wherein the glass frit mesh number is greater than 1500 mesh.
6. The silicone material adhesive according to claim 1, wherein the expansion coefficient adjuster is a silica sol solution.
7. A silicon material adhesive according to claim 6, wherein the expansion coefficient adjuster has a silica sol particle size of less than 50nm and a silica sol content of 20 to 40%.
8. The silicone material adhesive of claim 1, wherein the thickener is an aqueous solution of hydroxyethyl cellulose.
9. A method of preparing a silicone material adhesive as claimed in any one of claims 1 to 8, comprising the steps of:
adding a thickening agent into a solvent, and uniformly mixing;
weighing glass powder according to the mass requirement, adding the glass powder into a solvent with a thickening agent, and uniformly mixing;
and adding an expansion coefficient regulator into the solution added with the thickening agent and the glass powder, and uniformly mixing.
10. A method of using a silicone adhesive as defined in any one of claims 1 to 8, comprising the steps of:
coating the adhesive on the bonding surface of the silicon material part to be bonded;
bonding the bonding surfaces of the silicon material parts to be bonded, and forming preliminary bonding after the solvent of the bonding agent is volatilized;
putting the silicon material part into a high-temperature furnace for welding, wherein the welding temperature is 950-1100 ℃, and the adhesive is sintered and melted in the welding process to form adhesion with the silicon material;
the bonding surface of the silicon material part after cooling has an expansion coefficient of 2.3-2.7 multiplied by 10 -6 Bonding material per deg.C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211322087.5A CN115584212B (en) | 2022-10-27 | 2022-10-27 | Silicon material adhesive and preparation method and application method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211322087.5A CN115584212B (en) | 2022-10-27 | 2022-10-27 | Silicon material adhesive and preparation method and application method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115584212A true CN115584212A (en) | 2023-01-10 |
| CN115584212B CN115584212B (en) | 2023-11-03 |
Family
ID=84781653
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211322087.5A Active CN115584212B (en) | 2022-10-27 | 2022-10-27 | Silicon material adhesive and preparation method and application method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115584212B (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102730974A (en) * | 2012-06-08 | 2012-10-17 | 王双喜 | Slurry for preparation of glass fluorescent layer used for LED encapsulation |
| CN107459935A (en) * | 2016-06-03 | 2017-12-12 | 上海岱山电力科技股份有限公司 | A kind of air-tightness high temperature resistant silicate adhesive |
| CN108148510A (en) * | 2017-12-28 | 2018-06-12 | 苏州科技大学 | A kind of normal temperature self-drying type inorganic nano material adhesive |
| CN108219681A (en) * | 2018-01-15 | 2018-06-29 | 上海穗杉实业股份有限公司 | A kind of high-temperature seal adhesive and its preparation method and application |
| CN112898904A (en) * | 2021-01-25 | 2021-06-04 | 株洲世林聚合物有限公司 | High-temperature-resistant inorganic adhesive and preparation method thereof |
| WO2022067685A1 (en) * | 2020-09-30 | 2022-04-07 | Materion Precision Optics (Shanghai) Limited | High temperature resistant binder |
-
2022
- 2022-10-27 CN CN202211322087.5A patent/CN115584212B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102730974A (en) * | 2012-06-08 | 2012-10-17 | 王双喜 | Slurry for preparation of glass fluorescent layer used for LED encapsulation |
| CN107459935A (en) * | 2016-06-03 | 2017-12-12 | 上海岱山电力科技股份有限公司 | A kind of air-tightness high temperature resistant silicate adhesive |
| CN108148510A (en) * | 2017-12-28 | 2018-06-12 | 苏州科技大学 | A kind of normal temperature self-drying type inorganic nano material adhesive |
| CN108219681A (en) * | 2018-01-15 | 2018-06-29 | 上海穗杉实业股份有限公司 | A kind of high-temperature seal adhesive and its preparation method and application |
| WO2022067685A1 (en) * | 2020-09-30 | 2022-04-07 | Materion Precision Optics (Shanghai) Limited | High temperature resistant binder |
| CN112898904A (en) * | 2021-01-25 | 2021-06-04 | 株洲世林聚合物有限公司 | High-temperature-resistant inorganic adhesive and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115584212B (en) | 2023-11-03 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US3669693A (en) | Germania-silica glasses and method of coating | |
| JP2009066528A (en) | Zeolite separation membrane, its manufacturing method, and sealant | |
| CN115584212A (en) | Silicon material adhesive and preparation method and use method thereof | |
| CN115196981A (en) | Silica-based ceramic core and preparation method thereof | |
| CN115029101A (en) | Environment-friendly energy-saving heat-insulating sealant and preparation method and application thereof | |
| CN114276152A (en) | Adhesive for tape casting of low-temperature co-fired ceramic material and preparation method thereof | |
| JPH07108786B2 (en) | Lead-zinc-borosilicate glass | |
| KR100197471B1 (en) | Silica glass jig | |
| US7989373B2 (en) | Hermetic sealing material | |
| US6248680B1 (en) | Low temperature burnout screen printing frit vehicles and pastes | |
| CN109161233B (en) | Surface coating slurry of platinum heating wire, preparation method and coating device thereof | |
| WO2023125299A1 (en) | Sealing glass gob for electrical connector and preparation method therefor | |
| CN113511813B (en) | Edge-coated glass for laser glass and preparation method and application thereof | |
| CN115286253A (en) | Preparation method of low-melting-point sealing glass powder for micro electronic mechanical system | |
| KR20150040838A (en) | Glass powder material and method for producing porous glassy film | |
| CN114988703A (en) | Sealing glass compound and preparation method and application method thereof | |
| JPH10180060A (en) | Composition for sealing inorganic separating membrane | |
| JPS58199751A (en) | Low melting point glass paste and nitrocellulose for low melting point glass paste | |
| CN111333330A (en) | Glass powder for sealing nickel-based superalloy and preparation and use methods thereof | |
| CN101289280B (en) | Iron-sealing microcrystalline glass | |
| JPH04222887A (en) | Insulating resin paste | |
| CN117023993A (en) | Leadless low-melting point glass-based sealing material, preparation method and application thereof | |
| JP2013177308A (en) | Crystalline bismuth-based material | |
| WO2023044837A1 (en) | Lead-free borosilicate glass material, and preparation method therefor and use thereof | |
| JPH04332754A (en) | Electrical insulating resin paste |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |