CN110591636B - Organic adhesive suitable for target bonding and preparation method thereof - Google Patents
Organic adhesive suitable for target bonding and preparation method thereof Download PDFInfo
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- 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
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- 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
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
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- 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
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- 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
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
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- 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
- C09J9/00—Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
- C09J9/02—Electrically-conducting adhesives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/085—Copper
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
The invention provides an organic adhesive for target bonding, which comprises the following components in parts by weight: 15-25 parts of organic bentonite, 40-60 parts of attapulgite, 500 parts of conductive powder, 15-25 parts of an active agent, 200 parts of modified bi-component room temperature vulcanized silicone rubber, 60-100 parts of a silane coupling agent, 40-60 parts of a diluent, 0.5-1 part of a platinum vulcanizing agent A component, 0.5-1 part of a platinum vulcanizing agent B component, 120 parts of polyethylene glycol 40080 and 3-7 parts of a defoaming agent; the modified bi-component room temperature vulcanized silicone rubber is an addition type bi-component room temperature vulcanized silicone rubber and phenolic resin, and the mass ratio of the addition type bi-component room temperature vulcanized silicone rubber to the phenolic resin is 5: 1 by physical mixing. The organic adhesive prepared by the invention can be cured at room temperature and can be rapidly cured by heating, and the cured organic adhesive has stable performance and can work at the temperature of 250 ℃ for a long time without change in performance. The target bonded by the adhesive prepared by the invention can stably work for a long time under high-temperature and high-power (more than or equal to 15KW/M) sputtering.
Description
Technical Field
The invention belongs to the technical field of organic silicon materials, and particularly relates to an organic adhesive suitable for target bonding and a preparation method thereof.
Background
With the progress of the PVD coating process and the updating of coating equipment, the requirements on the size and the use condition of the target are higher. For example, the length of a rotating target used in the Low-E glass industry has reached 3897mm, and the target with the specification can be realized by splicing and bonding multiple sections of targets obviously; for another example, the power of the AZO ceramic target used in the CIGS thin film photovoltaic industry has reached 26KW/m, and the chamber temperature needs to be heated to more than 200 ℃. The target material using indium as the bonding material has a melting point of only 156.5 ℃, so if the target material uses high power or the heating temperature of the cavity is higher than the melting point temperature of the indium, the risk of indium melting and target dropping exists, and the damage to the coating equipment and products is caused.
The prior patent CN106244093A discloses a room-temperature vulcanization addition type organic silicon pouring sealant composition, which comprises a basic polymer: is a linear organopolysiloxane having silicon-bonded vinyl groups at both ends, and has a dynamic viscosity value at 25 ℃ of 200mPa · s to 1000mPa · s; a crosslinking agent: is a hydrogenorganopolysiloxane having a dynamic viscosity value of 10mPa · s to 100mPa · s at 25 ℃; tackifier: is a polysiloxane with epoxy groups; as well as fillers, plasticizers, catalysts and inhibitors. The room temperature vulcanization addition type organic silicon pouring sealant composition improves the bonding force with a plastic base material and improves the waterproof sealing effect by adjusting the formula of a basic polymer and adding an epoxy organic silicon tackifier.
The prior art CN106753027A discloses a two-component conductive adhesive capable of being rapidly cured at low temperature. The composition comprises the following components in parts by weight: the conductive adhesive comprises a component A: comprises 200 parts of silver-plated copper powder 180-; the conductive adhesive component B: comprises 200 parts of silver-plated copper powder 180, 10-15 parts of reactive diluent, 20-30 parts of curing agent, 10-20 parts of accelerator and 5 parts of flatting agent or defoaming agent. The invention creatively silver-plates the copper powder for three times to prepare the copper powder with the high-compactness silver layer. The silver-plated copper powder is applied to conductive adhesive, the double-component quick low-temperature curing conductive adhesive is prepared, and meanwhile, the conductive adhesive is applied to a conductor prepared on a substrate, so that the conductor has high conductivity and good mechanical strength. The prior patent CN108659720A provides a conductive adhesive, which comprises the following raw materials: 30-40 parts of acrylic resin, 10-20 parts of conductive filler, 5-10 parts of photoinitiator, 5-6 parts of epoxy resin, 5-6 parts of latent curing agent and 2-3 parts of coupling agent. The invention can accelerate the curing reaction of the adhesive by the aid of ultraviolet irradiation, and simultaneously, the latent curing agent is added, so that the stability of the invention at room temperature is maintained, the storage time of the invention is prolonged, the curing temperature of the invention is reduced, the curing time of the invention is further shortened, the requirement of the invention on the film formation of the conductive adhesive is met, and the difficulty of manufacturing a miniature electronic device is reduced.
At present, organic adhesives with high electrical conductivity, heat conductivity and high shear strength are available in the market, the base materials are mostly thermosetting resins (such as epoxy resin, organic silicon resin, phenolic resin and the like), the base materials need to be heated and cured, and the cured base materials have the defects of high hardness, poor high temperature resistance and the like. When the conductive adhesive prepared by the base materials is used as a target material bonding, the target material is easy to crack in the curing process; when the coating is used at high temperature (not less than 200 ℃), some small molecular substances can be released, and the vacuum degree of the coating cavity is damaged.
Disclosure of Invention
The invention aims to provide a preparation method of an organic adhesive suitable for bonding a high-power-bearable sputtering target material, wherein the adhesive can be cured at room temperature and can also be heated to accelerate curing, the cured organic adhesive has good performances of electric conduction, heat conduction, shear strength, high-temperature stability and the like, the volume is not shrunk after curing, the elasticity is good, and the bonding rate of the target material and a back tube (accompanying tube) is high. The specific technical scheme is as follows:
an organic adhesive for target bonding comprises the following components in parts by weight: 15-25 parts of organic bentonite, 40-60 parts of attapulgite, 500 parts of conductive powder, 15-25 parts of an active agent, 200 parts of modified bi-component room temperature vulcanized silicone rubber, 60-100 parts of a silane coupling agent, 40-60 parts of a diluent, 0.5-1 part of a platinum vulcanizing agent A component, 0.5-1 part of a platinum vulcanizing agent B component, 120 parts of polyethylene glycol 40080 and 3-7 parts of a defoaming agent;
the modified bi-component room temperature vulcanized silicone rubber is an addition type bi-component room temperature vulcanized silicone rubber and phenolic resin according to the mass ratio of 5: 1, physically mixing to obtain the product;
the component A of the platinum vulcanizing agent is a diene cyclotetrasiloxane platinum (0) coordination compound;
the component B of the platinum vulcanizing agent is a Karster catalyst.
Specifically, the diluent is tetrahydrofuran.
Specifically, the defoaming agent is a siloxane defoaming agent.
Specifically, the conductive powder comprises metal powder and/or non-metal powder; the metal powder comprises one or more of gold, silver, copper, aluminum, zinc, iron, nickel, silver-coated copper and silver-coated nickel, and the non-metal powder comprises one or more of graphite, silver-coated graphite and silver-coated glass.
Specifically, the active agent is any one of polyoxyethylene oleyl ether type, ethoxylated methyl glucoside stearate type or polyoxyethylene sorbitan monolaurate.
Specifically, the silane coupling agent is any one of vinyl trimethoxy silane, gamma- (methacryloyloxy) propyl trimethoxy silane and gamma-epoxy propyl ether trimethoxy silane.
A preparation method of an organic adhesive suitable for target bonding specifically comprises the following steps:
(1) adding polyethylene glycol 400 and a catalyst into a silane coupling agent, adjusting the pH value to 9-10, stirring to uniformly mix and dissolve all phases, performing ultrasonic oscillation, and reacting in a water bath to obtain gel A;
(2) adding a diluent into the gel A obtained in the step (1) to dissolve the gel A, then adding modified double-component room temperature vulcanized silicone rubber, and stirring to obtain slurry I for later use;
(3) spraying and granulating the attapulgite and the conductive powder to obtain a composite conductive filler, adding the composite conductive filler, the organic bentonite and the active agent into the slurry I obtained in the step (2), and stirring to obtain a slurry II for later use;
(4) adding a platinum vulcanizing agent A component and a defoaming agent into the slurry II obtained in the step (3), stirring, and removing bubbles in vacuum to obtain an organic conductive heat-conducting adhesive A component;
(5) adding a platinum vulcanizing agent B component and a defoaming agent into the slurry II obtained in the step (3), stirring, and removing bubbles in vacuum to obtain an organic conductive heat-conducting adhesive B component;
(6) mixing the component A of the organic electric-conductive heat-conducting adhesive obtained in the step (4) and the component B of the organic electric-conductive heat-conducting adhesive obtained in the step (5) according to a mass ratio of 1:1, mixing, stirring, and removing bubbles in vacuum to obtain the organic adhesive suitable for target bonding.
Specifically, the stirring mode in the step (1) is to stir for 2-4h at the rotating speed of 350r/min by using an electric stirrer.
Specifically, the ultrasonic oscillation time in the step (1) is 1-3h, and the temperature of the water bath is 30-40 ℃.
Specifically, the stirring mode in the step (2) is to use a magnetic stirrer to stir at a rotation speed of 188-.
Specifically, the stirring mode in the step (3) is to adopt a cross stirring blade stirrer to stir for 1-2 hours at the rotating speed of 150-.
Specifically, the preparation method of the composite conductive filler in the step (3) comprises the following steps: utilizing 0.4-1 wt% of conductive filler and 2: 1-5: 1, ball milling dispersion and surface modification are carried out on the attapulgite and the conductive powder by the nonionic surface modifier, and spherical particles are formed by a centrifugal spraying process.
Specifically, the stirring manner in the step (4) and the step (5) is to use a magnetic stirrer to stir at a rotation speed of 188-.
The invention has the following outstanding advantages:
(1) the conductive filling material can be metal powder such as gold, silver, copper, aluminum, zinc, iron, nickel, silver-coated copper, silver-coated nickel and the like, and can also be non-metal powder such as graphite, silver-coated glass and the like. Rich raw materials, wide selection range, low price and easy industrialization.
(2) The invention utilizes the efficient dispersant and the surface modifier to carry out ball milling dispersion and surface modification on the attapulgite and other nano conductive powder materials, and forms spherical particles by means of a centrifugal spraying process, thereby being beneficial to uniformly dispersing various conductive powder materials, being beneficial to forming stable suspension of various conductive powder components in an organic solvent and improving the conductive and heat-conducting properties of the colloid.
(3) The invention utilizes the characteristics of the organic bentonite, can adjust the viscosity of the mixed solution of the silane coupling agent and the polyethylene glycol 400, and forms a solvation film and a three-dimensional network structure on the surface of the conductive powder to support and prevent the particles from sinking, thereby ensuring the uniformity and stability of the conductive powder in the solution.
(4) The organic adhesive prepared by the invention can be cured at room temperature and can also be heated to realize rapid curing, and the cured organic adhesive has stable performance and can work at the temperature of 250 ℃ for a long time without change in performance. The target bonded by the adhesive prepared by the invention can stably work for a long time under high-temperature and high-power (more than or equal to 15KW/M) sputtering.
(5) The preparation process of the bi-component organic adhesive is simple, the equipment investment is low, and the industrial production is easy to realize; and the use is convenient, the components are uniformly mixed according to the mass ratio of 1:1, and the industrial application is convenient.
(6) The organic adhesive prepared by the invention does not generate polluting gas and dust in the using process, and is friendly to human body and environment.
Detailed Description
All the raw materials used in the present application are commercially available, for example:
the organic bentonite is purchased from organic bentonite GmbH of Anji Tianlong, Zhejiang;
attapulgite was purchased from national star attapulgite, ltd, Mingguang;
silver-coated copper powder was purchased from Beijing Deke island gold technologies, Inc.;
graphite powder was purchased from Beijing Germany island gold technologies, Inc.;
chloroplatinic acid was purchased from jin Wai New materials, Inc. of Jiangsu;
tetrahydrofuran was purchased from Asahan chemical Co., Ltd, Changzhou;
the addition type bi-component room temperature vulcanized silicone rubber is purchased from Hongmen silica gel technology Limited company in Shenzhen city;
phenolic resin was purchased from shanghai kelin chemical ltd;
polyethylene glycol 400 was purchased from Shanghai Shu chemical Co., Ltd;
polyoxyethylene sorbitan monolaurate was purchased from golden jeans, inc;
polyoxyethylene oleyl ether was purchased from Shanghai Jinjinle industries, Inc.;
ethoxylated methyl glucoside stearate was purchased from golden mosaic, inc;
vinyltrimethoxysilane was obtained from Shanghai Jincong industries, Ltd;
the two-component platinum vulcanizing agent is purchased from Shenzhen Shenlibang polymer materials GmbH; wherein the component A of the platinum vulcanizing agent is a diene cyclotetrasiloxane platinum (0) coordination compound; the platinum vulcanizing agent B component is a Karster catalyst;
gamma- (methacryloyloxy) propyltrimethoxysilane was obtained from golden mosaic, inc;
the silicone defoaming agent is purchased from Gnapu, four New science and technology applications research institute, Inc.
The formulations of the organic adhesives to which examples 1-4 of the present application refer are as follows:
the modified bi-component room temperature vulcanized silicone rubber is an addition type bi-component room temperature vulcanized silicone rubber and phenolic resin according to the mass ratio of 5: 1 by physical mixing.
The organic adhesive related to the embodiments 1-4 of the application is prepared by the following method:
(1) putting a silane coupling agent in a beaker, adding polyethylene glycol 400 and a catalyst, adjusting the pH value to 9-10, stirring for 1h by using an electric stirrer at the stirring speed of 300r/min to uniformly mix and dissolve all phases, sealing the solution, carrying out ultrasonic oscillation for 1h in an ultrasonic cleaning machine, and finally placing in a 35 ℃ water bath for reaction to obtain gel A;
(2) adding Tetrahydrofuran (THF) into the gel A to dissolve the THF, adding modified double-component room temperature vulcanized silicone rubber, and stirring in a magnetic stirrer at a rotating speed of 200r/min for 1h to obtain slurry I for later use;
(3) spraying and granulating the attapulgite and the conductive powder to prepare the composite conductive filler with excellent conductivity; putting the prepared composite conductive filler and organic bentonite into the slurry I obtained in the step (2), adding an active agent, fully stirring by using a cross stirring blade stirrer, wherein the stirring speed is 150r/min, and the stirring time is 1.5h, and then dividing the prepared slurry II into two parts of suspension slurry A and suspension slurry B with equal mass for later use;
(4) adding the platinum vulcanizing agent A component and a defoaming agent into the suspension slurry A obtained in the step (3), putting the suspension slurry A into a magnetic stirrer, stirring for 1h at the rotating speed of 188r/min, and defoaming the stirred slurry in vacuum to obtain the glue A of the organic electric-conductive heat-conducting adhesive;
(5) adding a platinum vulcanizing agent component B and a defoaming agent into the suspension slurry B obtained in the step (3), putting the suspension slurry B into a magnetic stirrer, stirring for 1h at the rotating speed of 188r/min, and defoaming the stirred slurry in vacuum to obtain a B glue of the organic electric-conductive heat-conducting adhesive;
(6) and (3) mixing the glue A and the glue B prepared in the steps (4) and (5) according to the mass ratio of 1: and 1, putting the mixture into a magnetic vacuum defoaming stirrer to be quickly stirred for 5 hours to obtain the organic electric-conduction heat-conduction adhesive suitable for target bonding.
Comparative example 1
In comparison with example 1, 20g of organobentonite was omitted in this comparative example, and the other steps and the weight of the raw material were not changed.
Comparative example 2
In this comparative example, the modified two-component room temperature vulcanizing silicone rubber was replaced with a room temperature vulcanizing silicone rubber, as compared with example 3, and the others were not changed.
Comparative example 3
Compared with example 3, the polyethylene glycol 400 is replaced by absolute ethyl alcohol in the comparative example, and the rest is not changed.
Comparative example 4
Compared with example 3, when the composite conductive filler is prepared by the comparative example, the dispersant and the surfactant are not added, and the rest is not changed.
Comparative example 5
Silver plating is carried out on copper powder for three times, particularly, 80nm spherical copper powder is selected to be a research object after silver plating, 200 parts of prepared silver-plated copper powder, 100 parts of epoxy resin and 15 parts of toluene are weighed, high-speed mechanical stirring is carried out for 10min, and a conductive adhesive component A is prepared; 180 parts of silver-plated copper powder prepared in example 1, 15 parts of 1, 4-butanediol diglycidyl ether, 30 parts of methyltetrahydrophthalic anhydride, 10 parts of triethanolamine and 5 parts of dibutyl phthalate were weighed and mechanically stirred at high speed for 10 minutes to prepare a conductive adhesive component B. Mixing the component A and the component B for 10 min.
Comparative example 6
30 parts of acrylic resin, 10 parts of modified copper powder, 5 parts of α -diethoxyacetophenone, 5 parts of epoxy resin, 5 parts of dicyandiamide and 2 parts of vinyl trimethoxy silane, wherein the particle size of the modified copper powder is 200 meshes, the modified copper powder is prepared by mixing a copper sulfate solution and polyvinylpyrrolidone to ensure that the concentration of copper sulfate is 1mol/L, introducing nitrogen as a protective atmosphere, adding a citric acid solution at 50 ℃ to adjust the pH of the system to be 6, reacting for 20min to obtain copper powder, mixing and ball-milling the copper powder and nano titanium nitride powder accounting for 2% of the addition amount of the copper powder, uniformly stirring 50 parts of ball-milled product, 5 parts of oleic acid, 1 part of curing agent and 5 parts of epoxy resin, and modifying the dicyandiamide by mixing ethylene diamine and dicyandiamide in equal mass, and heating for 4 hours at 120 ℃.
Experimental example 1
The organic electric-conductive and heat-conductive adhesives prepared in examples 1 to 4 and comparative examples 1 to 6 and suitable for target bonding were subjected to performance testing, wherein the sample size was Φ 30mm × 6mm, the curing condition was 100 ℃/1h, and the results are shown in the following table:
| test items | Example 1 | Example 2 | Example 3 | Example 4 |
| Curing time at 30 DEG C | ≤3h | ≤3h | ≤3h | ≤3.5h |
| Resistivity of | ≤5.7*10-2Ω.CM | ≤5.7*10-2Ω.CM | ≤5.7*10-2Ω.CM | ≤5.7*10-2Ω.CM |
| Coefficient of thermal conductivity | 6.0W/(M.K) | 6.0W/(M.K) | 6.0W/(M.K) | 6.0W/(M.K) |
| Hardness of | 59A | 59A | 56A | 55A |
| Shear strength at 100 ℃ | ≥1.2MPa | ≥1.2MPa | ≥1.0MPa | ≥1.0MPa |
| Shear strength at 250 ℃ | ≥1.2MPa | ≥1.2MPa | ≥1.0MPa | ≥1.0MPa |
| Volatilization at 100 deg.C/1 h | ≤1.1％ | ≤1.1％ | ≤1.3％ | ≤1.3％ |
| Volatilization at 250 deg.C/1 h | ≤1.1％ | ≤1.1％ | ≤1.3％ | ≤1.3％ |
The above table tests show that: the electric and heat conductive silicone adhesives prepared in the embodiments 1 to 4 have good electric and heat conductive performance and bonding strength, and the volatilization amount and the bonding strength do not change obviously under long-term baking at 250 ℃, namely the temperature resistance of the gelatin is excellent.
The test results in the table above show that: the electric and heat conducting performance and the bonding strength of the electric and heat conducting organic silicon adhesive prepared in the comparative example 1 are reduced to some extent, the volatilization amount is obviously increased under the long-term baking at 250 ℃, the bonding strength is obviously reduced, and the temperature resistance of the gelatin is poor. The main function of bentonite is to improve the suspension stability of conductive particles and other components in the colloid, and the high temperature stability of the colloid after curing. The hardness and the shear strength of the electric and heat conductive silicone adhesive prepared in the comparative example 2 are obviously increased. And the shearing strength is obviously increased under the long-term baking at 250 ℃, the bonding strength is obviously reduced, namely the elasticity of the gelatin is poor, and the service life of the target material can be greatly reduced in the later use of the target material. The volatilization amount of the electric and heat conductive organic silicon adhesive prepared in the comparative example 3 is obviously increased under long-term baking at 250 ℃, the bonding strength is obviously reduced, and the gelatin is unstable at high temperature and can release a large amount of small molecules, so that the vacuum degree of the target in the using process is influenced. The electric and heat conducting performance of the electric and heat conducting organic silicon adhesive prepared in the comparative example 4 is obviously reduced, the hardness of the colloid is increased, and the performance is unstable at high temperature, namely the electric and heat conducting performance and the hardness of the colloid are influenced by the composite electric and heat conducting filler. The conductive adhesives prepared in the comparative examples 5 and 6 contain epoxy resin, and the conductive powder only contains metal substances, so that the hardness is high, the high-temperature volatilization amount is large, and the vacuum degree of a coating cavity can be damaged.
Experimental example 2:
using the adhesives prepared in examples 1-4 and comparative examples 1-66, a zinc aluminum oxide (AZO) rotary target of 3191mm length was bonded according to the rotary target bonding method described in the national patent CN 201810818156.9 (a rotary target that can withstand high power sputtering and a method for preparing the same). The method comprises the following steps:
(1) selecting a stainless steel back tube with the outer diameter of 133 +/-0.2 mm and the length of 3191 +/-1 mm and 12 sections of AZO tubular targets, and processing the stainless steel back tube and the AZO tubular targets into required shapes according to the requirements of a drawing. Cleaning the back tube and the AZO ceramic target material for 5-15min by using an ultrasonic cleaning machine, and wiping the outer surface of the back tube and the inner hole of the target material by using absolute ethyl alcohol after drying;
(2) horizontally fixing the stainless steel back pipe on a rotary bracket, and then winding a metal copper mesh (wherein the width of the copper mesh is 5-20cm, the thickness is 0.1-0.2mm, and the mesh number is 30-100 meshes) on the outer wall of the stainless steel back pipe 1, wherein the lap joint width of each circle of metal mesh sheets is about 5 cm; the outer surface and the end surface of the AZO tube target are pasted with high-temperature adhesive tapes, and the inner wall is lined with a layer of metal copper mesh with the thickness of 0.1-0.2 mm;
(3) brushing the prepared organic conductive heat-conducting adhesive on the surface of the stainless steel back tube and the inner wall of the target, and then sleeving the AZO tube target on the back tube, wherein the fit clearance between the inner wall of the target and the outer wall of the back tube is 0.3-0.8 mm;
(4) and starting the rotating bracket at the rotating speed of 5 revolutions per minute, starting a heating source to heat the bonded target material at the heating temperature of 90 ℃ for 4 hours. Turning off the heating source until the target material is cooled to room temperature;
(5) and cleaning the high-temperature adhesive tape on the surface of the AZO target material and redundant adhesive and other pollutants in the abutted seams of the adjacent target materials, and finishing the bonding of the AZO rotary target material which can bear high-power sputtering (not less than 15 KW/M).
The target material is subjected to 16000KWH (power supply power is 20KW/M) on Low-E glass magnetron sputtering coating equipment, the target material using the adhesive in the embodiments 1-4 has no abnormal problems of target material nodulation, cracking, arcing and the like, and the electric and heat conductive organic adhesive prepared by the invention is completely suitable for binding high-power sputtering target materials; the targets using the adhesives in comparative examples 1-6 have the abnormal problems of a small amount of target nodulation, cracking, arcing and the like.
The above detailed description is specific to one possible embodiment of the present invention, and the embodiment is not intended to limit the scope of the present invention, and all equivalent implementations or modifications without departing from the scope of the present invention should be included in the technical solutions of the present invention.
Claims (10)
1. An organic adhesive suitable for target bonding comprises the following components in parts by weight: 15-25 parts of organic bentonite, 40-60 parts of attapulgite, 500 parts of conductive powder, 15-25 parts of an active agent, 200 parts of modified bi-component room temperature vulcanized silicone rubber, 60-100 parts of a silane coupling agent, 40-60 parts of a diluent, 0.5-1 part of a platinum vulcanizing agent A component, 0.5-1 part of a platinum vulcanizing agent B component, 120 parts of polyethylene glycol 40080 and 3-7 parts of a defoaming agent;
the modified bi-component room temperature vulcanized silicone rubber is an addition type bi-component room temperature vulcanized silicone rubber and phenolic resin according to the mass ratio of 5: 1, physically mixing to obtain the product;
the component A of the platinum vulcanizing agent is a diene cyclotetrasiloxane platinum (0) coordination compound;
the component B of the platinum vulcanizing agent is a Karster catalyst.
2. The organic adhesive suitable for target bonding according to claim 1, wherein the diluent is tetrahydrofuran.
3. The organic adhesive suitable for target bonding according to claim 1, wherein the defoaming agent is a siloxane defoaming agent.
4. The organic adhesive suitable for target bonding according to claim 1, wherein the conductive powder comprises metal powder and/or non-metal powder; the metal powder comprises one or more of gold, silver, copper, aluminum, zinc, iron, nickel, silver-coated copper and silver-coated nickel, and the non-metal powder comprises one or more of graphite, silver-coated graphite and silver-coated glass.
5. The organic adhesive suitable for target bonding according to claim 1, wherein the active agent is any one of polyoxyethylene oleyl ether type, ethoxylated methyl glucoside stearate type or polyoxyethylene sorbitan monolaurate.
6. The organic adhesive suitable for target bonding according to claim 1, wherein the silane coupling agent is any one of vinyltrimethoxysilane, gamma- (methacryloyloxy) propyltrimethoxysilane, or gamma-epoxypropylethertrimethoxysilane.
7. The method for preparing the organic adhesive suitable for target bonding according to claim 1, comprising the following steps:
(1) adding polyethylene glycol 400 and a catalyst into a silane coupling agent, adjusting the pH value to 9-10, stirring to uniformly mix and dissolve all phases, performing ultrasonic oscillation, and reacting in a water bath to obtain gel A;
(2) adding a diluent into the gel A obtained in the step (1) to dissolve the gel A, then adding modified double-component room temperature vulcanized silicone rubber, and stirring to obtain slurry I for later use;
(3) spraying and granulating the attapulgite and the conductive powder to obtain a composite conductive filler, adding the composite conductive filler, the organic bentonite and the active agent into the slurry I obtained in the step (2), and stirring to obtain a slurry II for later use;
(4) adding a platinum vulcanizing agent A component and a defoaming agent into the slurry II obtained in the step (3), stirring, and removing bubbles in vacuum to obtain an organic conductive heat-conducting adhesive A component;
(5) adding a platinum vulcanizing agent B component and a defoaming agent into the slurry II obtained in the step (3), stirring, and removing bubbles in vacuum to obtain an organic conductive heat-conducting adhesive B component;
(6) mixing the component A of the organic electric-conductive heat-conducting adhesive obtained in the step (4) and the component B of the organic electric-conductive heat-conducting adhesive obtained in the step (5) according to a mass ratio of 1:1, mixing, stirring, and removing bubbles in vacuum to obtain the organic adhesive suitable for target bonding.
8. The preparation method according to claim 7, wherein the stirring manner in the step (1) is stirring for 2-4h at a rotation speed of 350r/min by using an electric stirrer; the ultrasonic oscillation time is 1-3h, and the temperature of the water bath is 30-40 ℃.
9. The preparation method as claimed in claim 7, wherein the stirring manner in step (2) is stirring for 0.5-1h at a rotation speed of 188-.
10. The preparation method as claimed in claim 7, wherein the stirring manner in step (3) is stirring for 1-2h at a rotation speed of 150-300r/min by using a cross-shaped blade stirrer; the stirring mode in the step (4) and the step (5) is to adopt a magnetic stirrer to stir for 0.5-1h at the rotating speed of 188-.
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