CN113637439B - Glue applied to packaging of core optical devices of optical modules and preparation method thereof - Google Patents

Glue applied to packaging of core optical devices of optical modules and preparation method thereof Download PDF

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Publication number
CN113637439B
CN113637439B CN202110898924.8A CN202110898924A CN113637439B CN 113637439 B CN113637439 B CN 113637439B CN 202110898924 A CN202110898924 A CN 202110898924A CN 113637439 B CN113637439 B CN 113637439B
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glue
stirring
speed
shell powder
parts
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CN113637439A (en
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黄勇
高小燕
廖静
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Sichuan Tianyi Comheart Telecom Co Ltd
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Sichuan Tianyi Comheart Telecom Co Ltd
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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
    • C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
    • 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
    • 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
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24—Acids; Salts thereof
    • C08K3/26—Carbonates; Bicarbonates
    • C08K2003/265—Calcium, strontium or barium carbonate

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

The invention discloses glue applied to packaging of an optical module core optical device and a preparation method thereof; the preparation method comprises the following steps: adding 3 parts of first glue (formed by mixing 353ND (A/B) glue according to the mass ratio of 10: 1) into 10 parts of second glue (formed by mixing 353ND-T (A/B) glue according to the mass ratio of 10: 1) to be fully mixed, and then sequentially adding 0.6 part of modified shell powder, 0.7 part of organic bentonite and 1 part of benzyl glycidyl ether to be fully mixed and defoamed to obtain the adhesive. The glue has the advantages of proper fluidity, strong adhesion force and high stability, and is particularly suitable for coupling packaging between the receiving TO and the Base of BOSA optical devices.

Description

Glue applied to packaging of core optical devices of optical modules and preparation method thereof
Technical Field
The invention relates to the field of optical device packaging, in particular to glue applied to optical module core optical device packaging and a preparation method thereof.
Background
The optical module is composed of an optoelectronic device, a functional circuit, an optical interface and the like, wherein the optoelectronic device comprises a transmitting device and a receiving device. The light emitting portion is called a TOSA, the light receiving portion is called a ROSA, and the two portions are together called a BOSA. The glue adhesion effect of the optical device directly affects the overall reliability and service life of the optical device.
In the prior art, there are various glues for adhering optical devices, such as 353ND (A/B), 353ND-T (A/B), etc. When an optical device is actually adhered, 353ND (A/B) or 353ND-T (A/B) glue is singly adhered, and because the two glue are two-component glue, when the adhesive is singly used, the two-component glue needs to be mixed according to the mass ratio of 10.
When the 353ND (A/B) glue is singly adhered, the 353ND glue has too strong fluidity, and easily leaks into and dirties the structure diagrams in the filter and the base during glue dispensing; the 353ND-T (A/B) glue is poor in flowability when used alone, and cannot flow into a proper position during glue dispensing, so that the adhesion effect is poor. And the two glues have poor and unstable pulling resistance in the process of independently adhering the optical device, so that the packaged PD-TO and BOSA are easily separated from each other, the overall performance of the device is invalid, and the device cannot work.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides glue applied to the packaging of core optical devices of an optical module and a preparation method thereof; the glue prepared by the preparation method has proper fluidity, strong adhesive force and high stability, and is particularly suitable for coupling packaging between the receiving TO and Base of BOSA optical devices.
The purpose of the invention is realized by the following technical scheme: the glue applied to packaging of the core optical device of the optical module comprises the following raw materials in parts by weight: 2-4 parts of first glue and 9-11 parts of second glue; wherein the first glue is formed by mixing 353ND (A/B) glue according to the mass ratio of 10: 1; the second glue is formed by mixing 353ND-T (A/B) glue according to the mass ratio of 10: 1.
Further, the glue comprises the following raw materials in parts by weight: 2-4 parts of first glue, 9-11 parts of second glue, 0.5-0.7 part of modified shell powder, 0.6-0.8 part of modified organic bentonite and 0.9-1.1 part of benzyl glycidyl ether.
The preparation process of the modified shell powder comprises the following steps:
A. crushing and grinding the shell until the particle size is 0.2-0.4mm to obtain shell powder;
B. roasting the shell powder for 18-28h at 800-900 ℃, and then crushing the shell powder to 50-70nm.
The preparation process of the modified organic bentonite comprises the following steps: calcining organic bentonite at 600-700 deg.C for 6-8 hr, and pulverizing to 200-300nm.
Further, the glue comprises the following raw materials in parts by weight: 3 parts of first glue, 10 parts of second glue, 0.6 part of modified shell powder, 0.7 part of modified organic bentonite and 1 part of benzyl glycidyl ether.
In the scheme, 353ND (A/B) glue is mixed independently and has strong liquidity, and easily leaks into and dirties the filter plate and the internal structure of the base during glue dispensing; and 353ND-T (A/B) glue is poor in flowability when used alone, and cannot flow into a proper position during glue dispensing, so that the adhesion effect is poor. And the pulling resistance of the two glues in the process of independently adhering the optical device is not ideal, so that the packaged PD-TO and BOSA are easily separated from each other, and the overall performance of the device is failed. In the mixing process, a large amount of peculiar smell can be emitted by the glue, the glue is very easy to layer and is unstable after centrifugal treatment, and the prepared glue contains a large amount of bacteria, such as escherichia coli, staphylococcus aureus, salmonella and the like, so that the performance of the glue is unstable during packaging. Aiming at the technical problems, the modified shell powder is added in the glue blending process, the modified shell powder can adsorb partial peculiar smell generated by the glue, the adverse effect on human health caused by generation of a large amount of peculiar smell in the use process of the glue is reduced, meanwhile, the modified shell powder can adsorb bacteria in the glue, and the reduction of the bacteria can ensure that the performance of the glue after solidification is reliable and stable. In addition, when 353ND (A/B) glue and 353ND-T (A/B) glue are mixed, layering phenomenon can occur after centrifugation, so that a stabilizing agent needs to be added into the components, and meanwhile, in order to prevent finished glue from being hung upside down during glue dispensing, modified organic bentonite is added, the modified organic bentonite can expand rapidly in the glue, and meanwhile, the strong adsorbability of the modified organic bentonite can adsorb the modified shell powder, so that the modified shell powder and bentonite stone can be jointly used as a framework of the glue to support the glue after solidification, and the adhesiveness of the glue is further improved. In addition, because the modified organic bentonite has certain thickening property, and the addition of the modified shell powder can also reduce the fluidity of the glue, the glue cannot flow into a proper position during glue dispensing, and the adhesion effect is reduced, therefore, an active diluent, namely benzyl glycidyl ether, needs to be added to dilute the glue, so that the finished glue has proper fluidity, and meanwhile, the addition of the benzyl glycidyl ether can enhance the expansion degree of the bentonite in the glue, further improve the stability of the glue, and prevent the glue from layering. Meanwhile, the modified organic bentonite can also be used as a thixotropic agent, so that the glue can generate thixotropy, solid-liquid separation in a centrifugal process and sagging in a glue dispensing process are prevented, and the positioning and stability of the glue are further improved.
The second purpose of the invention is to provide a glue preparation method applied to optical module core optical device packaging, which comprises the following specific steps:
s1: mixing 353ND (A/B) glue according to the mass ratio of 10:1, and fully stirring to obtain first glue; mixing 353ND-T (A/B) glue according to the mass ratio of 10:1, and fully stirring to obtain second glue;
s2: taking materials according to the weight part ratio, adding 9-11 parts of the second glue into a reaction kettle, then adding 2-4 parts of the first glue, primarily stirring, then adding 0.5-0.7 part of modified shell powder, performing first vacuum stirring, then continuously adding 0.6-0.8 part of modified organic bentonite and 0.9-1.1 part of benzyl glycidyl ether, and performing second vacuum stirring to obtain a glue semi-finished product;
s3: and defoaming the semi-finished glue to obtain a finished glue.
Preferably, the stirring speed of S1 is 120-180r/min, and the stirring time is 2-4min. Under the condition, 353ND (A/B) glue and 353ND-T (A/B) glue can be respectively and fully mixed, if the time and the stirring speed are too low, the glue is not fully stirred, the adhesion effect of the glue exerted in the subsequent process is influenced, and if the stirring time is too long, the glue is sticky and the fluidity is reduced.
Preferably, in the step S2, 10 parts of the second glue is added into a reaction kettle, 3 parts of the first glue is added for primary stirring, 0.6 part of modified shell powder is added for primary vacuum stirring, 0.7 part of modified organic bentonite and 1 part of benzyl glycidyl ether are continuously added for secondary vacuum stirring, and a semi-finished glue is prepared;
preferably, in S2: in the primary stirring process, the second glue is firstly added into the first glue in batches within 25-30S, stirring is carried out while adding, the stirring speed is 120-180r/min, and after the second glue is added, vacuum stirring is carried out for 1-3min, wherein the stirring speed is 120-180r/min; in the first vacuum stirring process, the stirring speed is 240-360r/min, and the stirring time is 2-4min; in the second vacuum stirring process, low-speed stirring is firstly adopted, the stirring speed is 120-180r/min, and the stirring time is 1-3min; then stirring at high speed of 240-300r/min for 2-4min; in the step S2, the temperature in the reaction kettle is kept at 20-30 ℃. Add first glue in the second glue in batches, can increase the area of contact of first glue and second glue, improve the mixing efficiency of the two, can also reduce the two simultaneously and produce the bubble in mixing process, promote the stability ability of glue. And in the second vacuum stirring process, low-speed stirring is firstly adopted, and then high-speed stirring is adopted, so that the glue is easier to generate thixotropy, solid-liquid separation in the subsequent centrifugal process and sagging in the glue dispensing process are prevented, and the positioning and stability of the glue are improved. Simultaneously, adopt vacuum stirring, can get rid of the peculiar smell that glue produced in mixing process, reduce it and cause the injury to the human body in the use, simultaneously, can also tentatively get rid of the bubble in the glue, reduce follow-up centrifugal defoaming process's time, improve the use ageing of glue.
Preferably, the preparation process of the modified shell powder comprises the following steps:
A. crushing and grinding the modified shell until the particle size is 0.2-0.4mm to obtain modified shell powder;
B. roasting the modified shell powder for 18-28h at 800-900 ℃, and then crushing the shell powder to 50-70nm.
The modified shell powder is in a porous fibrous double-helix structure, and can effectively remove peculiar smell and bacteria in the glue, such as escherichia coli, staphylococcus aureus, salmonella and the like, so that the corrosion of the bacteria to the glue is reduced, the performance of the glue after being cured is reliable and stable, and the service life of the glue is prolonged. Meanwhile, the modified shell powder with the particle size of 50-70nm can be better dispersed in the glue, so that the adhesion of the glue is further improved.
Preferably, the preparation process of the modified organic bentonite comprises the following steps: roasting the modified organic bentonite at 600-700 deg.c for 6-8 hr, and crushing to 200-300nm. The modified organic bentonite has the advantages of increasing the porosity, loosening the structure and increasing the specific surface area, so that the adsorption performance is improved to a certain extent, the adsorbability of the modified shell powder is improved, the stability of the modified shell powder and the modified shell powder as a skeleton is enhanced, and the stability of the glue is further enhanced.
Preferably, the defoaming step is: and centrifuging the primary glue finished product at the centrifugal rotating speed of 900-1200r/min for 6-8min.
Preferably, the centrifugal speed is 1000r/min, and the centrifugal time is 7min.
The invention has the beneficial effects that:
1. the glue is prepared by mixing a first glue [ formed by mixing 353ND (A/B) glue according TO the mass ratio of 10:1 ] and a second glue [ formed by mixing 353ND-T (A/B) glue according TO the mass ratio of 10:1 ] according TO the weight ratio of 3.
2. The modified shell powder which is in a porous fibrous double-helix structure is added, so that bacteria in the glue can be effectively adsorbed, such as escherichia coli, staphylococcus aureus, salmonella and the like, corrosion of the bacteria to the glue is reduced, the performance of the glue after solidification is reliable and stable, and the service life of the glue is prolonged; meanwhile, the modified shell powder can adsorb toxic peculiar smell in the glue, so that the influence on human health caused by volatilization of the peculiar smell in the use process of the glue is prevented; in addition, the modified shell powder can be better dispersed in glue, and the adhesion of the glue is further improved.
3. By adding the modified organic bentonite, the modified shell powder and the bentonite are jointly used as a framework of the glue by rapidly expanding in the glue and having a strong adsorption effect on the modified shell powder, and the glue is supported after being cured, so that the adhesion of the glue is further improved. Meanwhile, the modified organic bentonite can also be used as a thixotropic agent, so that the glue can generate thixotropy, solid-liquid separation in a centrifugal process and sagging in a glue dispensing process are prevented, and the positioning and stability of the glue are further improved.
4. By adding the benzyl glycidyl ether serving as the active diluent, the glue can be diluted, the influence of the reduction of the fluidity and the adhesion of the glue caused by the addition of the glue into the modified shell powder and the modified organic bentonite can be improved, and the finished glue has proper fluidity; meanwhile, the addition of benzyl glycidyl ether can enhance the swelling degree of bentonite in the glue, further improve the stability of the glue and prevent the glue from layering.
5. Through adopting the vacuum stirring, can get rid of the peculiar smell that glue produced in mixing process, reduce it and cause the injury to the human body in the use, simultaneously, can also tentatively get rid of the bubble in the glue, reduce the time of follow-up centrifugal defoaming process, improve the use ageing of glue. The stability and the life of glue are further improved, and the phenomenon that the quality of an optical device is influenced by a void point caused by bubbles in the glue dispensing process is prevented.
In summary, the following steps: the glue prepared by the invention has proper fluidity, stronger adhesive force and higher stability, can achieve stronger pulling resistance and adhesiveness compared with singly using 353ND (A/B) glue and 353ND-T (A/B) glue, and is particularly suitable for coupling packaging between the receiving TO and Base of BOSA optical devices.
In addition, in the prior art, although it is difficult to achieve a strong effect of adhering the optical device by using 353ND (a/B) glue and 353ND-T (a/B) glue alone, few people mix them because it is difficult to control the amount of the two glues and it is impossible to predict whether the mixed glue can produce a significant effect. The preparation process of the invention has the advantages of multiple medicine addition and multiple operation processes, and if the process is not optimized, the operation process takes a lot of time, so that the actual use time of the glue is shortened. According to the invention, each operation step is optimized, the operation time is shortened, the prepared glue can exert high adhesion and strong drawing resistance, the use time of the glue can be maximized, and the method has remarkable progress.
Detailed Description
The technical solution of the present invention is further described in detail with reference to the following examples, but the scope of the present invention is not limited to the following.
1. Examples and comparative examples (all materials used in this application are commercially available chemical materials; all equipment used are commercially available equipment)
Example 1
S1: mixing 353ND (A/B) glue according to a mass ratio of 10:1, and fully stirring to obtain first glue, wherein the stirring speed is 120r/min, and the stirring time is 4min; mixing 353ND-T (A/B) glue according to the mass ratio of 10:1, and fully stirring to obtain second glue; wherein the stirring speed is 120r/min, and the stirring time is 4min;
s2: adding 90g of second glue into a reaction kettle, then adding 20g of first glue, and carrying out preliminary stirring, specifically, adding the first glue into the second glue in batches within 30S while stirring at a stirring speed of 120r/min, and carrying out vacuum stirring for 3min after the first glue is added, wherein the stirring speed is 120r/min; then adding 5g of modified shell powder to carry out first vacuum stirring, wherein the stirring speed is 120r/min, and the stirring time is 4min; then, continuously adding 6g of modified organic bentonite and 9g of benzyl glycidyl ether to carry out second vacuum stirring to obtain a semi-finished glue; in the second vacuum stirring process, low-speed stirring is firstly adopted, the stirring speed is 120r/min, and the stirring time is 3min; then, high-speed stirring is adopted, the stirring speed is 240r/min, and the stirring time is 4min. In the step S2, the temperature in the reaction kettle is kept at 20-30 ℃.
S3: placing the primary glue finished product into a centrifugal machine for centrifugal defoaming treatment to obtain a finished glue product; wherein the centrifugal speed is 900r/min, and the centrifugal time is 8min.
And directly using the prepared glue finished product for packaging the optical device TO receive the TO and the BASE, and then heating and curing at 120 ℃ for 40min TO finish packaging and curing.
Example 2
S1: mixing 353ND (A/B) glue according to a mass ratio of 10:1, and fully stirring to obtain first glue, wherein the stirring speed is 180r/min, and the stirring time is 2min; mixing 353ND-T (A/B) glue according to the mass ratio of 10:1, and fully stirring to obtain second glue; wherein the stirring speed is 180r/min, and the stirring time is 2min;
s2: adding 110g of second glue into a reaction kettle, then adding 40g of first glue, and carrying out preliminary stirring, specifically, adding the first glue into the second glue in batches within 30S while stirring at a stirring speed of 180r/min, and carrying out vacuum stirring for 1min after the first glue is added, wherein the stirring speed is 180r/min; then adding 5g of modified shell powder to carry out first vacuum stirring, wherein the stirring speed is 180r/min, and the stirring time is 2min; then, continuously adding 6g of modified organic bentonite and 9g of benzyl glycidyl ether to carry out second vacuum stirring to obtain a semi-finished glue; in the second vacuum stirring process, low-speed stirring is firstly adopted, the stirring speed is 180r/min, and the stirring time is 1min; then stirring at high speed of 300r/min for 2min. In the step S2, the temperature in the reaction kettle is kept at 20-30 ℃.
S3: placing the primary glue finished product into a centrifugal machine for centrifugal defoaming treatment to obtain a finished glue product; wherein the centrifugal speed is 1100r/min, and the centrifugal time is 6min.
And directly using the prepared glue finished product for packaging the TO and BASE of the optical device, and then heating and curing at 120 ℃ for 40min TO complete packaging and curing.
Example 3
S1: mixing 353ND (A/B) glue according to a mass ratio of 10:1, and fully stirring to obtain first glue, wherein the stirring speed is 150r/min, and the stirring time is 3min; mixing 353ND-T (A/B) glue according to the mass ratio of 10:1, and fully stirring to obtain second glue; wherein the stirring speed is 150r/min, and the stirring time is 3min;
s2: adding 100g of second glue into a reaction kettle, then adding 30g of first glue, and carrying out preliminary stirring, specifically, adding the first glue into the second glue in batches within 30S while stirring at a stirring speed of 150r/min, and carrying out vacuum stirring for 2min after the first glue is added, wherein the stirring speed is 150r/min; then 5g of modified shell powder is added for primary vacuum stirring, the stirring speed is 150r/min, and the stirring time is 3min; then, continuously adding 6g of modified organic bentonite and 9g of benzyl glycidyl ether to carry out second vacuum stirring to obtain a semi-finished glue; in the second vacuum stirring process, low-speed stirring is firstly adopted, the stirring speed is 150r/min, and the stirring time is 2min; then, high-speed stirring is adopted, the stirring speed is 270r/min, and the stirring time is 3min. In the step S2, the temperature in the reaction kettle is kept at 20-30 ℃.
S3: placing the primary glue finished product into a centrifugal machine for centrifugal defoaming treatment to obtain a finished glue product; wherein the centrifugal speed is 1000r/min, and the centrifugal time is 7min.
And directly using the prepared glue finished product for packaging the TO and BASE of the optical device, and then heating and curing at 120 ℃ for 40min TO complete packaging and curing.
Example 4
S1: mixing 353ND (A/B) glue according to a mass ratio of 10:1, and fully stirring to obtain first glue, wherein the stirring speed is 150r/min, and the stirring time is 3min; mixing 353ND-T (A/B) glue according to the mass ratio of 10:1, and fully stirring to obtain second glue; wherein the stirring speed is 150r/min, and the stirring time is 3min;
s2: adding 100g of second glue into a reaction kettle, then adding 30g of first glue, and carrying out preliminary stirring, specifically, adding the first glue into the second glue in batches within 30S while stirring at a stirring speed of 150r/min, and carrying out vacuum stirring for 2min after the first glue is added, wherein the stirring speed is 150r/min; then 15g of modified shell powder is added for primary vacuum stirring, the stirring speed is 150r/min, and the stirring time is 3min; then, continuously adding 6g of modified organic bentonite and 9g of benzyl glycidyl ether to carry out second vacuum stirring to obtain a semi-finished glue; in the second vacuum stirring process, low-speed stirring is firstly adopted, the stirring speed is 150r/min, and the stirring time is 2min; then, high-speed stirring is adopted, the stirring speed is 270r/min, and the stirring time is 3min. In the step S2, the temperature in the reaction kettle is kept at 20-30 ℃.
S3: placing the primary glue finished product into a centrifugal machine for centrifugal defoaming treatment to obtain a finished glue product; wherein the centrifugal speed is 1000r/min, and the centrifugal time is 7min.
And directly using the prepared glue finished product for packaging the optical device TO receive the TO and the BASE, and then heating and curing at 120 ℃ for 40min TO finish packaging and curing.
Example 5
S1: mixing 353ND (A/B) glue according to a mass ratio of 10:1, and fully stirring to obtain first glue, wherein the stirring speed is 150r/min, and the stirring time is 3min; mixing 353ND-T (A/B) glue according to the mass ratio of 10:1, and fully stirring to obtain second glue; wherein the stirring speed is 150r/min, and the stirring time is 3min;
s2: adding 100g of second glue into a reaction kettle, then adding 30g of first glue, and carrying out preliminary stirring, specifically, adding the first glue into the second glue in batches within 30S while stirring at a stirring speed of 150r/min, and carrying out vacuum stirring for 2min after the first glue is added, wherein the stirring speed is 150r/min; then adding 5g of modified shell powder to carry out first vacuum stirring, wherein the stirring speed is 150r/min, and the stirring time is 3min; then, continuously adding 1g of modified organic bentonite and 9g of benzyl glycidyl ether to carry out second vacuum stirring to obtain a semi-finished glue; in the second vacuum stirring process, low-speed stirring is firstly adopted, the stirring speed is 150r/min, and the stirring time is 2min; then, high-speed stirring is adopted, the stirring speed is 270r/min, and the stirring time is 3min. In the step S2, the temperature in the reaction kettle is kept at 20-30 ℃.
S3: placing the primary glue finished product into a centrifugal machine for centrifugal defoaming treatment to obtain a finished glue product; wherein the centrifugal speed is 1000r/min, and the centrifugal time is 7min.
And directly using the prepared glue finished product for packaging the optical device TO receive the TO and the BASE, and then heating and curing at 120 ℃ for 40min TO finish packaging and curing.
Example 6
S1: mixing 353ND (A/B) glue according to a mass ratio of 10:1, and fully stirring to obtain first glue, wherein the stirring speed is 150r/min, and the stirring time is 3min; mixing 353ND-T (A/B) glue according to the mass ratio of 10:1, and fully stirring to obtain second glue; wherein the stirring speed is 150r/min, and the stirring time is 3min;
s2: adding 100g of second glue into a reaction kettle, then adding 30g of first glue, and carrying out preliminary stirring, specifically, adding the first glue into the second glue in batches within 30S while stirring at a stirring speed of 150r/min, and carrying out vacuum stirring for 2min after the first glue is added, wherein the stirring speed is 150r/min; then adding 5g of modified shell powder to carry out first vacuum stirring, wherein the stirring speed is 150r/min, and the stirring time is 3min; then, continuously adding 1g of modified organic bentonite and 15g of benzyl glycidyl ether to carry out second vacuum stirring to obtain a semi-finished glue; in the second vacuum stirring process, low-speed stirring is firstly adopted, the stirring speed is 150r/min, and the stirring time is 2min; then, high-speed stirring is adopted, the stirring speed is 270r/min, and the stirring time is 3min. In the step S2, the temperature in the reaction kettle is kept at 20-30 ℃.
S3: placing the primary glue finished product into a centrifugal machine for centrifugal defoaming treatment to obtain a finished glue product; wherein the centrifugal speed is 1000r/min, and the centrifugal time is 7min.
And directly using the prepared glue finished product for packaging the optical device TO receive the TO and the BASE, and then heating and curing at 120 ℃ for 40min TO finish packaging and curing.
Example 7
S1: mixing 353ND (A/B) glue according to a mass ratio of 10:1, and fully stirring to obtain first glue, wherein the stirring speed is 150r/min, and the stirring time is 3min; mixing 353ND-T (A/B) glue according to the mass ratio of 10:1, and fully stirring to obtain second glue; wherein the stirring speed is 150r/min, and the stirring time is 3min;
s2: adding 100g of second glue into a reaction kettle, then adding 30g of first glue, and carrying out preliminary stirring, specifically, adding the first glue into the second glue in batches within 30S while stirring at a stirring speed of 150r/min, carrying out vacuum stirring for 2min after the first glue is added, wherein the stirring speed is 150r/min, and then centrifuging the stirred mixed glue, wherein the centrifugal rotating speed is 1000r/min, and the centrifugal time is 7min.
And directly using the centrifuged glue for packaging the optical device TO receive the TO and the BASE, heating and curing at 120 ℃ for 40min, and completing packaging and curing.
Example 8
S1: mixing 353ND (A/B) glue according to a mass ratio of 10:1, and fully stirring to obtain first glue, wherein the stirring speed is 150r/min, and the stirring time is 2min; mixing 353ND-T (A/B) glue according to the mass ratio of 10:1, and fully stirring to obtain second glue; wherein the stirring speed is 150r/min, and the stirring time is 3min;
s2: adding 30g of second glue into a reaction kettle, then adding 30g of first glue, and carrying out preliminary stirring, specifically, adding the first glue into the second glue in batches within 30S while stirring at a stirring speed of 150r/min, carrying out vacuum stirring for 2min after the first glue is added, wherein the stirring speed is 150r/min, and then centrifuging the stirred mixed glue, wherein the centrifugal rotating speed is 1000r/min, and the centrifugal time is 7min. .
And directly using the centrifuged glue for packaging the optical device TO receive the TO and the BASE, heating and curing at 120 ℃ for 40min, and completing packaging and curing.
Example 9
S1: mixing 353ND (A/B) glue according to a mass ratio of 10:1, and fully stirring to obtain first glue, wherein the stirring speed is 150r/min, and the stirring time is 2min; mixing 353ND-T (A/B) glue according to the mass ratio of 10:1, and fully stirring to obtain second glue; wherein the stirring speed is 150r/min, and the stirring time is 2min;
s2: adding 100g of second glue into a reaction kettle, then adding 10g of first glue, and primarily stirring, specifically, adding the first glue into the second glue in batches within 30S while stirring at a stirring speed of 150r/min, after the first glue is added, carrying out vacuum stirring for 2min at a stirring speed of 150r/min, and then centrifuging the stirred mixed glue at a centrifugal speed of 1000r/min for 7min. .
And directly using the centrifuged glue for packaging the TO and BASE of the optical device, heating and curing at 120 ℃ for 40min, and completing packaging and curing.
Example 10
S1: mixing 353ND (A/B) glue according to the mass ratio of 10:1, and fully stirring to obtain first glue; mixing 353ND-T (A/B) glue according to the mass ratio of 10:1, and fully stirring to obtain second glue;
s2: and (3) freely stirring 30g of first glue and 100g of second glue (not according TO the primary stirring process of the embodiment 7), centrifuging the stirred mixed glue, directly using the centrifuged glue for receiving TO and BASE of the packaged optical device, heating and curing at 120 ℃ for 40min, and completing the packaging and curing.
Example 11
S1: mixing 353ND (A/B) glue according to a mass ratio of 10:1, and fully stirring to obtain first glue, wherein the stirring speed is 150r/min, and the stirring time is 3min; mixing 353ND-T (A/B) glue according to the mass ratio of 10:1, and fully stirring to obtain second glue; wherein the stirring speed is 150r/min, and the stirring time is 3min;
s2: and (3) freely mixing 100g of second glue, 30g of first glue, 5g of modified shell powder, 6g of modified organic bentonite and 9g of benzyl glycidyl ether, centrifuging the mixed glue after mixing is finished, directly using the centrifuged glue finished product for packaging an optical device TO receive TO and BASE, then heating and curing at 120 ℃ for 40min, and completing packaging and curing. Comparative example 1
After commercially available 353ND (A/B) glue is mixed according TO the proportion of 10.
Comparative example 2
After commercially available 353ND-T (A/B) glue is mixed according TO the ratio of 10.
2. Test detection and data analysis.
Tensile tests were conducted on examples 1-10 and comparative examples 1-2 and the results are shown in the following table:
wherein: PD tension standard value: is more than 15Kg.
Figure GDA0003878955410000091
Figure GDA0003878955410000101
As can be seen from examples 1-11 and comparative examples 1-2, the formulations and preparation processes in examples 1-3 are strictly in accordance with the invention, so that the prepared glue finished product has significant advantages in PD tension resistance, meanwhile, the flowability of the glue is proper, and the service life of the glue reaches the normal service time. Compared with the single use of 353ND (A/B) glue and 353ND-T (A/B) glue, the glue has positive effects on the pulling resistance and the flowability of the glue.
It can be seen from the comparison of examples 4-6 and example 3 that if shell powder, modified organobentonite and benzyl glycidyl ether are not added according to the weight ratio of the present invention, the obtained glue has almost no positive effect on the pull-out resistance, and the pull-out resistance level is equivalent to that of 353ND (A/B) glue and 353ND-T (A/B) glue which are used alone.
As can be seen from the comparison of examples 7-9, the first glue and the second glue were mixed separately and the ratio of 3: the drawing resistance of a glue finished product obtained by the mass ratio of 10 is far better than that of 1:1 and 1, and the drawing resistance is far better than that of 353ND (A/B) glue and 353ND-T (A/B) glue which are used independently; the tensile resistance of the glue which is not prepared according to the proportion of the invention is lower, even lower than that of the glue which is singly used for 353ND (A/B) glue and 353ND-T (A/B) glue.
Comparing example 7 with example 10, it can be seen that when the first glue and the second glue are in the same ratio, the glue prepared by the preparation process of the present invention has stronger pulling resistance and longer service life.
Comparing example 3 with example 11, it can be seen that when the formulation and the ratio of the present invention are adopted, the glue prepared according to the preparation process of the present invention has stronger pulling resistance and longer service life. Compared with glue prepared by only mixing the first glue and the second glue according to the formula disclosed by the invention, the drawing resistance is stronger.
In conclusion, the glue prepared according to the formula and the preparation process disclosed by the invention can play a remarkable role in the aspects of drawing resistance and use aging. However, it should be noted that, due to the characteristics of the glue, the prepared glue has a certain use time, and although the preparation process is optimized in the scheme to minimize the preparation time, the preparation process still consumes a certain time, so the scheme is more suitable for large-scale batch production occasions with short use time.
The foregoing is merely a preferred embodiment of the invention, it is to be understood that the invention is not limited to the forms disclosed herein, but is not intended to be exhaustive or to limit the invention to other embodiments, and to various other combinations, modifications, and environments and may be modified within the scope of the inventive concept as expressed herein, by the teachings or the skill or knowledge of the relevant art. And that modifications and variations may be effected by those skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.

Claims (7)

1. The glue for packaging the core optical device of the optical module is characterized by comprising the following raw materials in parts by weight: 2-4 parts of first glue, 9-11 parts of second glue, 0.5-0.7 part of modified shell powder, 0.6-0.8 part of modified organic bentonite and 0.9-1.1 part of benzyl glycidyl ether; wherein the first glue is formed by mixing 353ND (A/B) glue according to the mass ratio of 10: 1; the second glue is formed by mixing 353ND-T (A/B) glue according to the mass ratio of 10: 1;
the preparation process of the modified shell powder comprises the following steps:
A. crushing and grinding the shell until the particle size is 0.2-0.4mm to obtain shell powder;
B. roasting the shell powder for 18-28h at 800-900 ℃, and then crushing the shell powder to 50-70nm;
the preparation process of the modified organic bentonite comprises the following steps: the organic bentonite is roasted for 6-8h at 600-700 ℃, and then crushed to 200-300nm.
2. The glue applied to the packaging of the optical module core optical device in the claim 1 is characterized by comprising the following raw materials in parts by weight: 3 parts of first glue, 10 parts of second glue, 0.6 part of modified shell powder, 0.7 part of modified organic bentonite and 1 part of benzyl glycidyl ether.
3. A method for preparing the glue for the optical module core optical device package according to claim 1 or 2, wherein the method comprises the following steps:
s1: mixing 353ND (A/B) glue according to the mass ratio of 10:1, and fully stirring to obtain first glue; mixing 353ND-T (A/B) glue according to the mass ratio of 10:1, and fully stirring to obtain second glue;
s2: taking materials according to the weight part ratio, adding 9-11 parts of the second glue into a reaction kettle, then adding 2-4 parts of the first glue, primarily stirring, then adding 0.5-0.7 part of modified shell powder, performing first vacuum stirring, then continuously adding 0.6-0.8 part of modified organic bentonite and 0.9-1.1 part of benzyl glycidyl ether, and performing second vacuum stirring to obtain a glue semi-finished product;
s3: and defoaming the semi-finished glue to obtain a finished glue.
4. The method for preparing the glue for packaging the core optical device of the optical module according to claim 3, wherein the stirring speed of S1 is 120-180r/min, and the stirring time is 2-4min.
5. The method according to claim 3, wherein in the step S2, 10 parts of the second glue is added into a reaction kettle, 3 parts of the first glue are added, preliminary stirring is performed, 0.6 part of shell powder is added for first vacuum stirring, 0.7 part of organobentonite and 1 part of benzyl glycidyl ether are further added for second vacuum stirring, and a semi-finished glue is obtained.
6. The method for preparing the glue applied to the optical module core optical device package according to claim 3, wherein in the step S2: in the primary stirring process, the first glue is firstly added into the second glue in batches within 25-30S, stirring is carried out while adding, the stirring speed is 120-180r/min, and after the first glue is added, vacuum stirring is carried out for 1-3min, and the stirring speed is 120-180r/min; in the first vacuum stirring process, the stirring speed is 120-180r/min, and the stirring time is 2-4min; in the second vacuum stirring process, low-speed stirring is firstly adopted, the stirring speed is 120-180r/min, and the stirring time is 1-3min; then high-speed stirring is adopted, the stirring speed is 240-300r/min, and the stirring time is 2-4min; in the step S2, the temperature in the reaction kettle is kept at 20-30 ℃.
7. The method for preparing the glue applied to the packaging of the core optical device of the optical module in the claim 3, wherein the step of defoaming treatment is as follows: and centrifuging the semi-finished glue at the rotating speed of 900-1200r/min for 6-8min.
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