Luminescent perfluoroether elastomer composition as well as preparation method and application thereof

Abstract

The invention discloses a luminous perfluoroether elastomer composition which is prepared from the following raw materials in g: 90-110 parts of fluoroether rubber, 1-5 parts of a cross-linking agent and 1-10 parts of a composite luminous material. According to the invention, the CsPbBr3 perovskite quantum dot which is chemically synthesized is used as a core light-emitting component, so that the light-emitting efficiency is relatively high, and the light-emitting service life is relatively long. When the perovskite quantum dots are prepared into the composite luminescent material to be applied to the perfluoroether rubber, a self-luminous sealing elastomer can be obtained, and the use performance of a sealing element is not influenced. The prepared perfluoroether elastomer polymer has a uniform dispersion effect, can avoid adverse effects of luminescent perovskite quantum dots under the oxidation effect, and prevents fluorescence quenching caused by quantum dot aggregation or surface non-radiation center increase. The self-luminous perfluoroether elastomer has a self-luminous property, does not influence the mechanical properties of the perfluoroether elastomer, and still can keep a good sealing effect.

Description

Technical Field

[0001] The present invention relates to the field of polymer materials, and particularly relates to a luminescent perfluoroether elastomer composition, a preparation method and an application thereof. Background Art

[0002] Fluoroether elastomer seals are widely used in the semiconductor field. However, in actual applications, the internal space of semiconductor devices is small and the light is insufficient. When actually installing or overhauling, it is often necessary to rely on external light sources such as flashlights to ensure the correct installation and overhaul. Not only is the operation difficult, but there are also installation deviations caused by angle problems. Therefore, it is crucial to develop a self-luminous fluoroether elastomer seal for use in the semiconductor field.

[0003] Chinese Patent CN110408214B discloses a preparation method of super-biphobic fluorescent micro-nano spheres. Water-soluble starch is used as a carbon source to prepare fluorescent carbon quantum dots by ultrasonic method, and then KH570 is used to modify the carbon quantum dot / silica composite microspheres; then silicone rubber microspheres are prepared. Carbon quantum dot / silica / silicone rubber micro-nano spheres with good fluorescence effect and super-biphobic properties are obtained, but they are not applied to the encapsulation field and do not have the function of encapsulation materials. Chinese Patent CN113534311B discloses a quantum dot diffusion plate and a preparation method thereof. The surface treatment of quantum dots is carried out by surfactants and materials with small dielectric constants, reducing the aggregation phenomenon of quantum dots and improving the dispersion effect. However, the reaction process does not involve the vulcanization reaction of rubber and does not involve the problem of oxidation quenching during vulcanization. Summary of the Invention

[0004] In order to develop a self-luminous fluoroether elastomer seal for use in the semiconductor field, a first aspect of the present invention provides a luminescent perfluoroether elastomer composition. The preparation raw materials include 90-110 parts by weight of fluoroether rubber, 1-5 parts by weight of a crosslinking agent, and 1-10 parts by weight of a composite luminescent material.

[0005] As a preferred embodiment, the crosslinking agent is a compound containing phosphonium salts.

[0006] As a preferred embodiment, the preparation raw materials of the composite luminescent material include quantum dots, microporous composite materials and solvents, and the microporous composite material is a silica microporous material.

[0007] As a preferred embodiment, the preparation method of the composite luminescent material includes the following steps:

[0008] M1 Disperse 0.5-2 mg of quantum dots into 5-10 mL of n-hexane solvent, and mix evenly to obtain a quantum dot solution;

[0009] M2 disperses 10 - 50 parts by weight of the microporous composite material into the quantum dot solution prepared in step M1, ultrasonically treats it for 10 - 20 min, starts stirring, and stirs for 1 - 5 h to obtain a mixed solution;

[0010] M3 centrifuges the mixed solution prepared in step M2, and the bottom sediment is the composite luminescent material.

[0011] As a preferred embodiment, the centrifugation speed in step M3 is 5000 - 10000 rpm, and the centrifugation time is 3 - 8 min.

[0012] As a preferred embodiment, the centrifugation speed in step M3 is 8000 rpm, and the centrifugation time is 5 min.

[0013] As a preferred embodiment, the microporous composite material is a silica microporous composite material. Preferably, the microporous composite material is silica.

[0014] As a preferred embodiment, the quantum dot is a perovskite quantum dot, and the perovskite quantum dot is CsPbBr 3 nanocrystal.

[0015] As a preferred embodiment, the preparation raw materials of the CsPbBr 3 nanocrystal include 0.1 - 0.5 g of cesium source, 1 - 5 mL of oleic acid, 20 - 30 mL of fatty olefin, 1 - 5 mL of oleylamine, 0.1 - 0.3 g of lead bromide, and ethyl acetate.

[0016] Note: The weight unit is not limited to g, including but not limited to mg, g, kg, ton. The volume unit is not limited to mL, including but not limited to μL, mL, L.

[0017] As a preferred embodiment, the cesium source is cesium carbonate; the fatty olefin is octadecene.

[0018] As a preferred embodiment, the preparation method of the CsPbBr 3 nanocrystal includes the following steps:

[0019] N1 mixes 0.1 - 0.5 g of cesium source, 1 - 3 mL of oleic acid, and 3 - 5 mL of fatty olefin, and performs a degassing treatment at 100 °C for 3 h to obtain a uniformly dissolved cesium source mixture;

[0020] N2 mixes 0.1 - 0.3 g of lead bromide, 2 - 4 mL of oleic acid, 1 - 5 mL of oleylamine, and 18 - 22 mL of fatty olefin, and performs a degassing treatment at 100 °C for 3 h to remove moisture and oxygen to obtain a uniformly dissolved lead bromide mixture;

[0021] Heat N3 to 150 - 200 °C, add the cesium source mixture to the lead bromide mixture, hold for 20 - 40 s, and then perform rapid quenching treatment in a water bath to obtain a system mixture;

[0022] Add ethyl acetate with a volume three times that of the system mixture to N4, perform centrifugal separation, centrifuge at 5000 - 10000 rpm for 3 - 8 min, and take the sediment as CsPbBr 3 nanocrystals.

[0023] As a preferred embodiment, the preparation method of the CsPbBr 3 nanocrystals comprises the following steps:

[0024] Mix 0.1 g of cesium source, 1 mL of oleic acid, and 4 mL of fatty olefin, and perform degassing treatment at 100 °C for 3 h to obtain a uniformly dissolved cesium source mixture;

[0025] Mix 0.28 g of lead bromide, 3 mL of oleic acid, 3 mL of oleylamine, and 20 mL of fatty olefin, and perform degassing treatment at 100 °C for 3 h to remove moisture and oxygen, obtaining a uniformly dissolved lead bromide mixture;

[0026] Heat to 180 °C, add the cesium source mixture to the lead bromide mixture, hold for 30 s, and then perform rapid quenching treatment in a water bath to obtain a system mixture;

[0027] Add ethyl acetate with a volume three times that of the system mixture to N4, perform centrifugal separation, centrifuge at 8000 rpm for 5 min, and take the sediment as CsPbBr 3 nanocrystals.

[0028] The CsPbBr 3 perovskite quantum dots prepared by the present invention are chemically synthesized, have high luminescence efficiency, and as the core luminescent component of a luminescent perfluoroether elastomer composition, have a long luminescence lifetime.

[0029] The inventors found during the experiment that when perovskite quantum dots are prepared into a composite luminescent material and applied to perfluoroether rubber, a self-luminescent sealing elastomer can be obtained without affecting the service performance of the seal. It is speculated that the possible reason is: by combining perovskite quantum dots with silica microporous materials, the perovskite quantum dots can be uniformly dispersed in the silica microporous materials, improving the dispersion stability of the perovskite quantum dots and avoiding agglomeration during subsequent rubber crosslinking. And the combination of perovskite quantum dots with silica microporous materials can protect the quantum dots from external environmental erosion, further extending the luminescence lifetime of the quantum dots.

[0030] The second aspect of the present invention provides a preparation method of a luminescent perfluoroether elastomer composition, comprising the following steps:

[0031] S1 Put the fluoroether rubber into an open mill. After passing through the rolls of the open mill 1 - 5 times, add the composite luminescent material.

[0032] S2 Cut and knead the rubber on both sides, and after mixing evenly, add the crosslinking agent. Then cut and knead the rubber on both sides again, mix evenly, and adjust the roll gap to conduct thin passing 5 - 10 times.

[0033] S3 Adjust the roll gap and take out the sheet to obtain the luminescent perfluoroether elastomer composition.

[0034] As a preferred embodiment, the roll gap of the open mill in step S1 is 0.5 - 0.8 mm, the roll gap is adjusted to 0.1 - 0.3 mm in step S2, and the roll gap is adjusted to 0.8 - 1.2 mm in step S3.

[0035] As a preferred embodiment, the roll gap of the open mill in step S1 is 0.6 mm, the roll gap is adjusted to 0.1 mm in step S2, and the roll gap is adjusted to 1.0 mm in step S3.

[0036] The applicant further found that in the mixing process, a wider roll gap is first adopted and then a narrower roll gap is used, and the dispersion effect of the fluoroether elastomer polymer prepared is more uniform. During the mixing and rubber cutting process, the narrower roll gap further promotes the uniform dispersion of the composite luminescent material.

[0037] The third aspect of the present invention provides an application of the luminescent perfluoroether elastomer composition, and the luminescent perfluoroether elastomer composition is applied to the field of semiconductor packaging.

[0038] As a preferred embodiment, the luminescent perfluoroether elastomer composition is made into a seal through a vulcanization process, and the vulcanization process includes the following steps:

[0039] H1 Put the luminescent perfluoroether elastomer composition into a mold, place the mold in a flat vulcanizer for primary vulcanization. The temperature of the primary vulcanization is 150 - 200 °C, the vulcanization pressure is 5 - 15 MPa, and the vulcanization time is 10 - 20 min to obtain a primary vulcanized product.

[0040] H2 Let the primary vulcanized product stand at room temperature for 5 - 10 h, and then place it in an oven for secondary vulcanization to obtain a seal.

[0041] As a preferred embodiment, the vulcanization process includes the following steps:

[0042] H1 Put the luminescent perfluoroether elastomer composition into a mold, place the mold in a flat vulcanizer for primary vulcanization. The temperature of the primary vulcanization is 180 °C, the vulcanization pressure is 10 MPa, and the vulcanization time is 15 min to obtain a primary vulcanized product.

[0043] The primary vulcanizate of H2 is allowed to stand at room temperature for 8 h and then placed in an oven for secondary vulcanization to obtain the seal.

[0044] As a preferred embodiment, the oven program for secondary vulcanization in step H2 is as follows: the oven temperature is raised from 25°C to 250 - 300°C over a heating time of 5 - 10 h, then held at 250 - 300°C for 10 - 20 h, and then cooled to 25°C.

[0045] As a preferred embodiment, the oven program for secondary vulcanization in step H2 is as follows: the oven temperature is raised from 25°C to 290°C over a heating time of 8 h, then held at 290°C for 16 h, and then cooled to 25°C.

[0046] The inventors adopted a two-step vulcanization process in the vulcanization step. First, vulcanize at 180°C for 15 min, and then slowly raise the temperature to 290°C in the oven and vulcanize for 16 h. This can avoid the adverse effects of the luminescent perovskite quantum dots under oxidation, resulting in quantum dot aggregation or an increase in surface non-radiative centers, causing fluorescence quenching. The two-step vulcanization reaction also ensures excellent mechanical properties of the vulcanized rubber.

[0047] Compared with the prior art, the present invention has the following beneficial effects:

[0048] (1) The luminescent perfluoroether elastomer composition of the present invention uses chemically synthesized CsPbBr 3 perovskite quantum dots as the core luminescent component, having a relatively high luminescence efficiency and a relatively long luminescence lifetime.

[0049] (2) The luminescent perfluoroether elastomer composition of the present invention prepares the perovskite quantum dots into a composite luminescent material and applies it to perfluoroether rubber, so that a self-luminescent sealing elastomer can be obtained without affecting the service performance of the seal.

[0050] (3) The luminescent perfluoroether elastomer composition of the present invention first uses a relatively wide roll gap and then a relatively narrow roll gap during the mixing process. The prepared perfluoroether elastomer polymer has a relatively uniform dispersion effect, further promoting the dispersion uniformity of the composite luminescent material.

[0051] (4) The luminescent perfluoroether elastomer composition of the present invention adopts a two-step vulcanization process in the vulcanization step. First, vulcanize at 180°C for 15 min, and then slowly raise the temperature to 290°C in the oven and vulcanize for 16 h. This can avoid the adverse effects of the luminescent perovskite quantum dots under oxidation, resulting in quantum dot aggregation or an increase in surface non-radiative centers, causing fluorescence quenching.

[0052] (5) The luminescent perfluoroether elastomer composition of the present invention has self-luminescent properties without affecting the mechanical properties of the perfluoroether elastomer and can still maintain a good sealing effect. Brief Description of the Drawings

[0053] Figure 1 Physical pictures of the seals prepared for Example 1, left: under natural light, right: under ultraviolet light.

[0054] Figure 2 Physical pictures of the seals prepared for Example 2, left: under natural light, right: under ultraviolet light.

[0055] Figure 3 Physical pictures of the seals prepared for Example 3, left: under natural light, right: under ultraviolet light.

[0056] Figure 4 Physical pictures of the seals prepared for Example 4, left: under natural light, right: under ultraviolet light.

[0057] Figure 5 Physical pictures of the seals prepared for Example 5, left: under natural light, right: under ultraviolet light

[0058] Figure 6 Physical pictures of the seals prepared for Example 6, left: under natural light, right: under ultraviolet light

[0059] Figure 7 Physical pictures of the seals prepared for Example 7, left: under natural light, right: under ultraviolet light

[0060] Figure 8 Physical pictures of the seals prepared for Example 8, left: under natural light, right: under ultraviolet light Detailed Description of the Invention

[0061] Example 1

[0062] A luminescent perfluoroether elastomer composition, the raw materials for preparation include 100 parts by weight of fluoroether rubber, 1.2 parts of crosslinking agent, and 1 part of composite luminescent material.

[0063] The fluoroether rubber is purchased from Solvay, grade 1055B.

[0064] The crosslinking agent is purchased from 3M TM Dyneon TM , grade PFE 03C.

[0065] The preparation method of the composite luminescent material includes the following steps:

[0066] M1 Disperse 1 mg of quantum dots into 8 mL of n-hexane, mix evenly to obtain a quantum dot solution;

[0067] M2 disperses 30 g of the microporous composite material into the quantum dot solution prepared in step M1, ultrasonically treats it for 15 min, starts stirring, and stirs for 5 h to obtain a mixed solution;

[0068] M3 centrifuges the mixed solution prepared in step M2, and the bottom sediment is the composite luminescent material.

[0069] In the said step M3, the centrifugation speed is 8000 rpm and the centrifugation time is 5 min.

[0070] The said microporous composite material is silica.

[0071] The said quantum dots are CsPbBr 3 perovskite quantum dots.

[0072] The said CsPbBr 3 The preparation method of the perovskite quantum dots includes the following steps:

[0073] N1 mixes 0.1 g of cesium source, 1 mL of oleic acid, and 4 mL of octadecene, conducts a degassing treatment at 100 °C for 3 h to obtain a uniformly dissolved cesium source mixture;

[0074] N2 mixes 0.28 g of lead bromide, 3 mL of oleic acid, 3 mL of oleylamine, and 20 mL of octadecene, conducts a degassing treatment at 100 °C for 3 h to remove moisture and oxygen, and obtains a uniformly dissolved lead bromide mixture;

[0075] N3 raises the temperature to 180 °C, adds the cesium source mixture to the lead bromide mixture, holds for 30 s, and then conducts a rapid quenching treatment in a water bath to obtain a system mixture;

[0076] N4 adds ethyl acetate with a volume three times that of the system mixture, conducts centrifugal separation, centrifuges at 8000 rpm for 5 min, and takes the sediment as CsPbBr 3 perovskite quantum dots.

[0077] The said cesium source is cesium carbonate; the said octadecene is octadecene.

[0078] A preparation method of a luminescent perfluoroether elastomer composition includes the following steps:

[0079] S1 puts the fluoroether rubber into an open mill, after passing through the rolls of the open mill 3 times, adds the composite luminescent material;

[0080] S2 cuts and turns the rubber on the left and right for mixing, after mixing evenly, adds a crosslinking agent, cuts and turns the rubber on the left and right for mixing evenly, and adjusts the roll gap to thin pass 8 times;

[0081] S3 adjusts the roll gap and sheets out to obtain the luminescent perfluoroether elastomer composition.

[0082] In step S1, the roll gap of the open mill is 0.6 mm. In step S2, the roll gap is adjusted to 0.1 mm. In step S3, the roll gap is adjusted to 1.0 mm.

[0083] An application of a luminescent perfluoroether elastomer composition, wherein the luminescent perfluoroether elastomer composition is made into a seal through a vulcanization process, and the vulcanization process includes the following steps:

[0084] H1 Put the luminescent perfluoroether elastomer composition into a mold, place the mold in a flat vulcanizer for primary vulcanization. The temperature of the primary vulcanization is 180 °C, the vulcanization pressure is 10 MPa, and the vulcanization time is 15 min to obtain a primary vulcanized product.

[0085] H2 Let the primary vulcanized product stand at room temperature for 8 h, and then place it in an oven for secondary vulcanization to obtain a seal.

[0086] In step H2, the oven program for secondary vulcanization is as follows: the oven temperature is raised from 25 °C to 290 °C, the heating time is 8 h, then it is maintained at 290 °C for 16 h, and then cooled to 25 °C.

[0087] Example 2

[0088] A luminescent perfluoroether elastomer composition, the preparation raw materials include 100 parts by weight of fluoroether rubber, 1.2 parts of crosslinking agent, and 1.5 parts of composite luminescent material.

[0089] The remaining implementation manners are the same as those in Example 1.

[0090] Example 3

[0091] A luminescent perfluoroether elastomer composition, the preparation raw materials include 100 parts by weight of fluoroether rubber, 1.2 parts of crosslinking agent, and 3.0 parts of composite luminescent material.

[0092] The remaining implementation manners are the same as those in Example 1.

[0093] Example 4

[0094] A perfluoroether elastomer composition, the preparation raw materials include 100 parts by weight of fluoroether rubber and 1.2 parts of crosslinking agent.

[0095] The fluoroether rubber is purchased from Solvay, and the grade is 1055B.

[0096] The crosslinking agent is purchased from 3M TM Dyneon TM with the grade of PFE 03C.

[0097] A preparation method of a perfluoroether elastomer composition includes the following steps:

[0098] S1 Put the fluoroether rubber into an open mill, pass it through the rolls of the open mill 3 times, and add the crosslinking agent;

[0099] S2 Cut and knead the rubber on both sides, after mixing evenly, adjust the roll gap and thin pass 8 times;

[0100] S3 Adjust the roll gap and take out the sheet to obtain the perfluoroether elastomer composition.

[0101] In step S1, the roll gap of the open mill is 0.6 mm, in step S2, the roll gap is adjusted to 0.1 mm, and in step S3, the roll gap is adjusted to 1.0 mm.

[0102] An application of the perfluoroether elastomer composition, the perfluoroether elastomer composition is made into a seal through a vulcanization process, and the vulcanization process includes the following steps:

[0103] H1 Put the perfluoroether elastomer composition into a mold, place the mold in a flat vulcanizer for primary vulcanization, the temperature of the primary vulcanization is 180 °C, the vulcanization pressure is 10 MPa, and the vulcanization time is 15 min to obtain a primary vulcanized product;

[0104] H2 Let the primary vulcanized product stand at room temperature for 8 h, then put it in an oven for secondary vulcanization to obtain a seal.

[0105] In step H2, the oven program for secondary vulcanization is: the oven temperature rises from 25 °C to 290 °C, the heating time is 8 h, then it is kept at 290 °C for 16 h, and then it is cooled to 25 °C.

[0106] Example 5

[0107] A luminescent perfluoroether elastomer composition, the preparation raw materials include 100 parts by weight of fluoroether rubber, 1.2 parts of crosslinking agent, and 0.5 parts of quantum dots.

[0108] The fluoroether rubber is purchased from Solvay, and the grade is 1055B.

[0109] The crosslinking agent is purchased from 3M TM Dyneon TM , and the grade is PFE 03C.

[0110] The quantum dots are prepared by the preparation method of CsPbBr 3 perovskite quantum dots in Example 1.

[0111] A preparation method of a luminescent perfluoroether elastomer composition, including the following steps:

[0112] S1 Put the fluoroether rubber into an open mill, after passing it through the rolls of the open mill 3 times, add the quantum dots;

[0113] For S2, cut and knead the rubber on both sides, add the crosslinking agent after mixing evenly, cut and knead the rubber on both sides again, mix evenly, and adjust the roll gap to thin out 8 times;

[0114] S3 Adjust the roll gap and take out the sheet to obtain the luminescent perfluoroether elastomer composition.

[0115] In the step S1, the roll gap of the open mill is 0.6 mm, in the step S2, the roll gap is adjusted to 0.1 mm, and in the step S3, the roll gap is adjusted to 1.0 mm.

[0116] An application of the luminescent perfluoroether elastomer composition, the luminescent perfluoroether elastomer composition is made into a seal through a vulcanization process, and the vulcanization process includes the following steps:

[0117] H1 Put the luminescent perfluoroether elastomer composition into a mold, place the mold in a flat vulcanizer for primary vulcanization, the temperature of the primary vulcanization is 180 °C, the vulcanization pressure is 10 MPa, and the vulcanization time is 15 min to obtain a primary vulcanized product;

[0118] H2 Let the primary vulcanized product stand at room temperature for 8 h, and then place it in an oven for secondary vulcanization to obtain a seal.

[0119] In the step H2, the oven program for secondary vulcanization is: the oven temperature is raised from 25 °C to 290 °C, the heating time is 8 h, then it is kept at 290 °C for 16 h, and then it is cooled to 25 °C.

[0120] Example 6

[0121] A luminescent perfluoroether elastomer composition, the preparation raw materials include 100 parts by weight of fluoroether rubber, 1.2 parts of crosslinking agent, and 1.0 part of quantum dots.

[0122] The rest of the implementation methods are the same as those in Example 5.

[0123] Example 7

[0124] A luminescent perfluoroether elastomer composition, the preparation raw materials include 100 parts by weight of fluoroether rubber, 1.2 parts of crosslinking agent, and 1.0 part of silica.

[0125] The fluoroether rubber is purchased from Solvay, and the grade is 1055B.

[0126] The crosslinking agent is purchased from 3M TM Dyneon TM , and the grade is PFE 03C.

[0127] The silica is purchased from Evonik, and the grade is A380.

[0128] A preparation method of a luminescent perfluoroether elastomer composition, including the following steps:

[0129] S1 Put the fluoroether rubber into an open mill. After passing through the rolls of the open mill 3 times, add silica.

[0130] S2 Cut and knead the rubber from left to right. After mixing evenly, add the crosslinking agent, cut and knead the rubber from left to right, mix evenly, and adjust the roll gap to thin out 8 times.

[0131] S3 Adjust the roll gap and take out the sheet to obtain the luminescent perfluoroether elastomer composition.

[0132] In step S1, the roll gap of the open mill is 0.6 mm. In step S2, the roll gap is adjusted to 0.1 mm. In step S3, the roll gap is adjusted to 1.0 mm.

[0133] An application of the luminescent perfluoroether elastomer composition, wherein the luminescent perfluoroether elastomer composition is made into a seal through a vulcanization process. The vulcanization process includes the following steps:

[0134] H1 Put the luminescent perfluoroether elastomer composition into a mold, place the mold in a flat vulcanizer for primary vulcanization. The temperature of the primary vulcanization is 180 °C, the vulcanization pressure is 10 MPa, and the vulcanization time is 15 min to obtain a primary vulcanized product.

[0135] H2 Let the primary vulcanized product stand at room temperature for 8 h, then place it in an oven for secondary vulcanization to obtain a seal.

[0136] In step H2, the oven program for secondary vulcanization is as follows: the oven temperature rises from 25 °C to 290 °C, the heating time is 8 h, then it is kept at 290 °C for 16 h, and then it is cooled to 25 °C.

[0137] Example 8

[0138] A luminescent perfluoroether elastomer composition, the preparation raw materials include 100 parts by weight of fluoroether rubber, 1.2 parts of crosslinking agent, 0.5 part of quantum dots, and 1.0 part of silica.

[0139] The fluoroether rubber is purchased from Solvay, grade 1055B.

[0140] The crosslinking agent is purchased from 3M TM Dyneon TM , grade PFE 03C.

[0141] The silica is purchased from Evonik, grade A380.

[0142] The quantum dots are prepared by using the preparation method of CsPbBr 3 perovskite quantum dots in Example 1.

[0143] A preparation method of a luminescent perfluoroether elastomer composition, including the following steps:

[0144] In step S1, the fluoroether rubber is put into an open mill. After passing through the rolls of the open mill 3 times, quantum dots are added.

[0145] In step S2, cut and knead the rubber on both sides and turn it over for kneading. After mixing evenly, silica is added. Then cut and knead the rubber on both sides and turn it over for kneading. After mixing evenly, a crosslinking agent is added. Then cut and knead the rubber on both sides and turn it over for kneading until evenly mixed. Adjust the roll gap and thin out by passing through 8 times.

[0146] In step S3, adjust the roll gap and take out the sheet to obtain a luminescent perfluoroether elastomer composition.

[0147] In step S1, the roll gap of the open mill is 0.6 mm. In step S2, the roll gap is adjusted to 0.1 mm. In step S3, the roll gap is adjusted to 1.0 mm.

[0148] An application of a luminescent perfluoroether elastomer composition. The luminescent perfluoroether elastomer composition is made into a seal through a vulcanization process. The vulcanization process includes the following steps:

[0149] In step H1, the luminescent perfluoroether elastomer composition is put into a mold. The mold is placed in a flat vulcanizer for primary vulcanization. The temperature of the primary vulcanization is 180 °C, the vulcanization pressure is 10 MPa, and the vulcanization time is 15 min to obtain a primary vulcanized product.

[0150] In step H2, the primary vulcanized product is left standing at room temperature for 8 h, and then placed in an oven for secondary vulcanization to obtain a seal.

[0151] In step H2, the oven program for secondary vulcanization is as follows: the oven temperature is raised from 25 °C to 290 °C, the heating time is 8 h, then it is held at 290 °C for 16 h, and then cooled down to 25 °C.

[0152] Example 9

[0153] A luminescent perfluoroether elastomer composition, the preparation raw materials include 100 parts by weight of fluoroether rubber, 1.2 parts of crosslinking agent, 0.5 part of peroxide, 0.5 part of quantum dots, and 1.0 part of silica.

[0154] The fluoroether rubber is purchased from Solvay, with the grade 1055B.

[0155] The crosslinking agent is purchased from 3M TM Dyneon TM , with the grade PFE 03C.

[0156] The peroxide is 2,5-bis(tert-butyl)-2,5-dimethylhexane.

[0157] The silica is purchased from Evonik, with the grade A380.

[0158] The quantum dots are CsPbBr in Example 1. 3 The perovskite quantum dots are prepared by a preparation method.

[0159] A method for preparing a luminescent perfluoroether elastomer composition comprises the following steps:

[0160] S1 puts the fluoroether rubber into an open mill, passes through the open mill rollers for 3 times, and then adds quantum dots;

[0161] S2: tap the rubber left and right, mix them evenly, add silicon dioxide, tap the rubber left and right, mix them evenly, add cross-linking agent and peroxide, tap the rubber left and right, mix them evenly, adjust the roller distance and pass 8 times;

[0162] S3 adjusts the roller distance to produce a sheet to obtain a luminescent perfluoroether elastomer composition.

[0163] In step S1, the roller distance of the mixing mill is 0.6 mm, in step S2, the roller distance is adjusted to 0.1 mm, and in step S3, the roller distance is adjusted to 1.0 mm.

[0164] An application of a luminescent perfluoroether elastomer composition, wherein the luminescent perfluoroether elastomer composition is subjected to a vulcanization process to form a sealing member, wherein the vulcanization process comprises the following steps:

[0165] H1: Put the luminescent perfluoroether elastomer composition into a mold, and place the mold in a flat vulcanizer for primary vulcanization. The primary vulcanization temperature is 180°C, the vulcanization pressure is 10MPa, and the vulcanization time is 15min to obtain a primary vulcanized product;

[0166] The primary vulcanized product is left to stand at room temperature with H2 for 8 hours, and then placed in an oven for secondary vulcanization to obtain a seal.

[0167] The oven program for the secondary vulcanization in step H2 is as follows: the oven temperature is raised from 25°C to 290°C for 8 hours, then maintained at 290°C for 16 hours, and then cooled to 25°C.

[0168] Performance Testing

[0169] 1. Hardness: refer to the Shore hardness of test examples 1-8 according to GB / T531.1-2008 standard.

[0170] 2. Luminous intensity: The sample was tested under the excitation of ultraviolet light (365 nm) using a German GOSSEN handheld illuminometer at a fixed distance of 10 cm.

[0171] 3. Luminous level: The highest luminous intensity corresponds to the highest level 10, using the following formula

[0172]

[0173] PL x : The measured luminous intensity corresponding to Example x, with the unit of lux.

[0174] PL max : The maximum luminous intensity of the example, with the unit of lux.

[0175] The test results are shown in Table 1.

[0176] Table 1

[0177] Shore A hardness Luminescence level / level Luminescence intensity (lux) Example 1 71 3 67 Example 2 72 8 163 Example 3 73 10 209 Example 4 70 1 20 Example 5 70 1 22 Example 6 71 1 23 Example 7 71 1 21 Example 8 71 1 22 Example 9 70 1 17

Claims

1. A luminescent perfluoroether elastomer composition, characterized in that: The raw materials for preparation include 90-110 parts of fluoroether rubber, 1-5 parts of cross-linking agent and 1-10 parts of composite luminescent material in parts by weight.

2. The luminescent perfluoroether elastomer composition according to claim 1, characterized in that: The raw materials for preparing the composite luminescent material include quantum dots, microporous composite material and solvent, and the microporous composite material is silicon oxide microporous material.

3. The luminescent perfluoroether elastomer composition according to claim 2, characterized in that: The preparation method of the composite luminescent material comprises the following steps: M1 disperses the quantum dots into the solvent and mixes them evenly to obtain a quantum dot solution; M2 disperses the microporous composite material into the quantum dot solution, performs ultrasonication for 10-20 min, starts stirring, and stirs for 1-5 h to obtain a mixed solution; M3 centrifuges the mixed solution, and the bottom sediment is the composite luminescent material.

4. The luminescent perfluoroether elastomer composition according to claim 3, characterized in that: In the step M3, the centrifugal speed is 5000-10000 rpm, and the centrifugal time is 3-8 min.

5. The luminescent perfluoroether elastomer composition according to claim 2, characterized in that: The quantum dots are perovskite quantum dots, and the perovskite quantum dots are CsPbBr3 nanocrystals.

6. A method for preparing the luminescent perfluoroether elastomer composition according to any one of claims 1 to 5, characterized in that: The following steps are involved: S1: put the fluoroether rubber into an open mill, pass the open mill roller 1-5 times, and then add the composite luminescent material; S2 taps the rubber left and right, mixes evenly, adds cross-linking agent, taps the rubber left and right, mixes evenly, adjusts the roller distance and passes thinly 5-10 times; S3 adjusts the roller distance to produce a sheet to obtain a luminescent perfluoroether elastomer composition.

7. The method for preparing the luminescent perfluoroether elastomer composition according to claim 6, characterized in that: In the step S1, the roller spacing of the mixing mill is 0.5-0.8 mm, in the step S2, the roller spacing is adjusted to 0.1-0.3 mm, and in the step S3, the roller spacing is adjusted to 0.8-1.2 mm.

8. An application of the luminescent perfluoroether elastomer composition according to any one of claims 1 to 5, characterized in that: The luminescent perfluoroether elastomer composition is applied in the field of semiconductor packaging.

9. The use of the luminescent perfluoroether elastomer composition according to claim 8, characterized in that: The luminescent perfluoroether elastomer composition is subjected to a vulcanization process to form a seal, wherein the vulcanization process comprises the following steps: H1: Put the luminescent perfluoroether elastomer composition into a mold, and place the mold in a flat vulcanizer for primary vulcanization. The primary vulcanization temperature is 150-200°C, the vulcanization pressure is 5-15MPa, and the vulcanization time is 10-20min to obtain a primary vulcanized product; H2 allows the primary vulcanized product to stand at room temperature for 5-10 hours, and then places it in an oven for secondary vulcanization to obtain a seal.

10. The use of the luminescent perfluoroether elastomer composition according to claim 9, characterized in that: The oven program for the secondary vulcanization in step H2 is: the oven temperature is increased from 25°C to 250-300°C for 5-10 hours, then maintained at 250-300°C for 10-20 hours, and then cooled to 25°C.

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