A mechanoluminescence composite material, a preparation method and application thereof

Abstract

The application belongs to the technical field of mechanoluminescence materials, and relates to a mechanoluminescence composite material and a preparation method and application thereof. The mechanoluminescence composite material provided by the application comprises an SLMPD / PDMS composite layer and a silicone rubber layer located on the upper and lower surfaces of the SLMPD / PDMS composite layer; the silicone rubber layer is composed of a silicone rubber E625A component and a silicone rubber E625B component. The mechanoluminescence composite material provided by the application has excellent tensile properties.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of mechanoluminescence materials, and relates to a mechanoluminescence composite material and a preparation method and application thereof. BACKGROUND

[0002] Mechanoluminescence materials can convert external mechanical stimuli, including impact, bending, extrusion, impact, stretching, into light signals without any complex circuit design. Therefore, mechanoluminescence materials have important research value and application potential in the fields of lighting display, advanced information storage, artificial intelligence skin, structural health monitoring, mechanical sensing, artificial intelligence and Internet of Things. Among them, the artificial intelligence skin, wearable devices and flexible sensor devices have higher requirements for the flexibility and sensitivity of the mechanoluminescence composite material. Since the silicone has the advantages of non-toxic, soft, good elasticity, high transparency, cold and high temperature resistance, tensile environmental protection and stable performance. Therefore, silicone can be used as a candidate for a composite material. Sr9LiMg(PO4)7:Dy 3+ The composite material SLMPD / PDMS formed by the combination of SLMPD and the conventional organic polymer polyorganosiloxane (PDMS) can emit bright yellow light under mechanical stimulation, and the light emission phenomenon can be maintained for a period of time after the mechanical stimulation is removed. However, the conventional composite material SLMPD / PDMS has limited tensile performance and is prone to breakage. SUMMARY

[0003] Therefore, the application provides a mechanoluminescence composite material and a preparation method and application thereof. The tensile performance of the mechanoluminescence composite material provided by the application is excellent.

[0004] In order to achieve the above purpose, the application provides the following technical solutions.

[0005] The application provides a mechanoluminescence composite material, which comprises an SLMPD / PDMS composite layer and an organic silicone rubber layer located on the upper and lower surfaces of the SLMPD / PDMS composite layer.

[0006] The organic silicone rubber layer is composed of organic silicone rubber E625 A and organic silicone rubber E625 B components.

[0007] Preferably, the single-layer thickness of the organic silicone rubber layer is 0.4-0.6 mm.

[0008] Preferably, the thickness of the SLMPD / PDMS composite layer is 0.4-0.6 mm.

[0009] The application further provides a preparation method of the mechanoluminescence composite material, comprising the following steps.

[0010] mixing the silicone rubber E625 A and the silicone rubber E625 B components, first curing and forming to obtain a silicone rubber layer;

[0011] fixing a SLMPD / PDMS composite material on the surface of the silicone rubber layer to form a SLMPD / PDMS composite layer;

[0012] mixing the silicone rubber E625 A and the silicone rubber E625 B components, and second curing and forming on the surface of the SLMPD / PDMS composite layer to obtain the mechanoluminescent composite material.

[0013] Preferably, the temperature of the first curing and forming and the second curing and forming is independently 55-70℃, and the time is 0.8-1.2h.

[0014] Preferably, the mass ratio of the silicone rubber E625 A and the silicone rubber E625 B is 1:1.

[0015] Preferably, the preparation of the SLMPD / PDMS composite material comprises the following steps:

[0016] mixing the SLMPD, the organosiloxane and the curing agent, and curing to obtain the SLMPD / PDMS composite material.

[0017] Preferably, the organosiloxane is SYLGARD 184 Silicone Elastomer Base.

[0018] Preferably, the mass ratio of the SLMPD, the organosiloxane and the curing agent is 0.8-1:1.5-2:0.13-0.18.

[0019] The application further provides the application of the mechanoluminescent composite material or the mechanoluminescent composite material prepared by the preparation method in intelligent sensing, flexible electronic skin and wearable devices.

[0020] The application provides a mechanoluminescent composite material, comprising a SLMPD / PDMS composite layer and a silicone rubber layer on the upper and lower surfaces of the SLMPD / PDMS composite layer; the silicone rubber layer is composed of a silicone rubber E625 A component and a silicone rubber E625 B component. BRIEF DESCRIPTION OF DRAWINGS

[0021] Figure 1 The XRD spectrum of the SLMPD fluorescent powder obtained in Example 1.

[0022] Figure 2The force-induced luminescence spectrum of the SLMPD / PDMS composite obtained in Comparative Example 1.

[0023] Figure 3 The force-induced luminescence spectrum of the SLMPD / PDMS composite obtained in Comparative Example 1.

[0024] Figure 4 The force-induced luminescence spectrum of the SG / SLMPD / PDMS / SG composite obtained in Example 1 at different tensile deformation.

[0025] Figure 5 The sensitivity and deformation comparison chart of the SG / SLMPD / PDMS / SG composite obtained in Example 1 and the SLMPD / PDMS composite obtained in Comparative Example 1. DETAILED DESCRIPTION

[0026] The present application provides a force-induced luminescence composite material, comprising a SLMPD / PDMS composite layer and a silicone rubber layer on the upper and lower surfaces of the SLMPD / PDMS composite layer.

[0027] The silicone rubber layer is composed of silicone rubber E625 A and silicone rubber E625 B components.

[0028] In the present application, the reagents used are all commercially available and well known to those skilled in the art, unless otherwise specified.

[0029] In the present application, the force-induced luminescence composite material comprises a SLMPD / PDMS composite layer and a silicone rubber layer on the upper and lower surfaces of the SLMPD / PDMS composite layer; the silicone rubber layer is composed of silicone rubber E625 A and silicone rubber E625 B components.

[0030] In the present application, the thickness of the silicone rubber layer is preferably 0.4-0.6 mm, more preferably 0.5 mm. In the present application, the thickness of the SLMPD / PDMS composite layer is preferably 0.4-0.6 mm, more preferably 0.5 mm.

[0031] In the present application, the silicone rubber layer is composed of silicone rubber E625 A and silicone rubber E625 B components, and the mass ratio of the silicone rubber E625 A and the silicone rubber E625 B is preferably 1:1.

[0032] The present application also provides a preparation method of the force-induced luminescence composite material described above, comprising the following steps:

[0033] After mixing silicone rubber E625 A and silicone rubber E625 B components, first curing forming is carried out to obtain a silicone rubber layer;

[0034] An SLMPD / PDMS composite layer is fixed on the surface of the silicone rubber layer to form an SLMPD / PDMS composite layer.

[0035] After mixing silicone rubber E625 A and silicone rubber E625 B components, second curing forming is carried out on the surface of the SLMPD / PDMS composite layer to obtain the mechanoluminescent composite material.

[0036] The present application mixes silicone rubber E625 A and silicone rubber E625 B components, and then carries out first curing forming to obtain a silicone rubber layer.

[0037] In the present application, before the first curing forming, a step of standing to remove bubbles is further included.

[0038] In the present application, the temperature of the first curing forming is preferably 55-70℃, and more preferably 60℃; and the time is preferably 0.8-1.2h, and more preferably 1h.

[0039] After obtaining the silicone rubber layer, the present application fixes an SLMPD / PDMS composite layer on the surface of the silicone rubber layer.

[0040] In the present application, the preparation of the SLMPD / PDMS composite material preferably includes the following steps:

[0041] SLMPD, organosiloxane and a curing agent are mixed and cured to obtain the SLMPD / PDMS composite material.

[0042] In the present application, the SLMPD (Sr9LiMg(PO4)7:Dy 3+ ) is prepared by the following steps: mixing strontium carbonate, lithium carbonate, magnesium oxide, ammonium dihydrogen phosphate and dysprosium oxide, and then carrying out first roasting to obtain a first roasting product; after second grinding of the first roasting product, second roasting is carried out to obtain the SLMPD.

[0043] The present application mixes strontium carbonate, lithium carbonate, magnesium oxide, ammonium dihydrogen phosphate and dysprosium oxide, and then carries out first roasting to obtain a first roasting product.

[0044] In the present application, the molar ratio of strontium carbonate and lithium carbonate is preferably 1.64-1.66:0.04-0.06, more preferably 1.65:0.05. In the present application, the molar ratio of lithium carbonate and magnesium oxide is preferably 0.04-0.06:0.05-0.07, more preferably 0.05:0.06. In the present application, the molar ratio of magnesium oxide and ammonium dihydrogen phosphate is preferably 0.05-0.07:1.08-1.10, more preferably 0.06:1.09. In the present application, the molar ratio of ammonium dihydrogen phosphate and dysprosium oxide is preferably 1.08-1.10:0.01-0.03, more preferably 1.09:0.02.

[0045] In the present application, the mixing is preferably wet grinding mixing; the medium of the wet grinding mixing is preferably ethanol. In the present application, after the wet grinding mixing, preferably, drying is further included. The present application does not specifically limit the drying, which can remove the ethanol in the wet grinding mixing process.

[0046] In the present application, the temperature of the first roasting is preferably 500-700℃, more preferably 600℃; the holding time is preferably 1-3h, more preferably 2h. In the present application, the heating rate for heating to the temperature of the first roasting is preferably 4-6℃ / min, more preferably 5℃ / min.

[0047] After obtaining the first roasting product, the present application second grinds the first roasting product, and then performs second roasting to obtain the SLMPD.

[0048] In the present application, the temperature of the second roasting is preferably 1100-1300℃, more preferably 1200℃; the holding time is preferably 3-5h, more preferably 4h. In the present application, the heating rate for heating to the temperature of the second roasting is preferably 4-6℃ / min, more preferably 5℃ / min.

[0049] In the present application, the organosiloxane is preferably SYLGARD 184 Silicone Elastomer Base provided by Dow Corning Corporation of the United States. In the present application, the particle size of the SLMPD is preferably 5-40μm, more preferably 30μm.

[0050] In the present application, the mass ratio of the SLMPD, the organosiloxane and the curing agent is preferably 0.8-1:1.5-2:0.13-0.18, more preferably 0.9:1.7-1.8:0.15-0.17. In the present application, the curing agent is preferably silicone resin solution (SYLGARD 184 Silicone Elastomer Curing Agent).

[0051] In the present application, the temperature of the second curing is preferably 55-70℃, more preferably 60℃; the time is preferably 0.8-1.2h, more preferably 1h.

[0052] The present application mixes the silicone rubber E625 A and the silicone rubber E625 B components, and then performs second curing molding on the surface of the SLMPD / PDMS composite layer to obtain the mechanoluminescence composite material.

[0053] In the present application, the conditions of the second curing molding are preferably the same as the first curing molding, which will not be repeated here.

[0054] The present application also provides the application of the mechanoluminescence composite material or the mechanoluminescence composite material prepared by the above-mentioned preparation method in intelligent sensing, flexible electronic skin and wearable devices.

[0055] The technical solutions provided by the present application will be described in detail below in combination with examples, but they should not be understood as limiting the scope of protection of the present application.

[0056] Example 1

[0057] 8.28mmol of strontium carbonate, 1mmol of lithium carbonate, 1mmol of magnesium oxide, 7mmol of ammonium dihydrogen phosphate and 0.36mmol of dysprosium oxide are mixed, the mixed powder is ground uniformly with the aid of ethanol, dried in an oven and then ground, loaded into a crucible, placed in a muffle furnace, calcined at 600℃ for 2h, and naturally cooled to obtain a first calcined product;

[0058] After the first calcined product is ground, the powder is placed in a muffle furnace and calcined at 1200℃ for 4h, and after natural cooling, the product is ground to a particle size of 5-40μm to obtain SLMPD.

[0059] Silicone rubber E625 A and silicone rubber E625 B are weighed according to a mass ratio of 0.5:0.5, mixed uniformly, poured into a mold, and left to stand to remove bubbles, and then heated at 60℃ for 1h to make the silicone first curing molding to obtain an organic silicon rubber layer.

[0060] SLMPD, organosiloxane (SYLGARD 184 Silicone Elastomer Base) and silicone resin solution (SYLGARD 184 Silicone Elastomer Curing Agent) are weighed according to a mass ratio of 0.8:1.5:0.13, mixed uniformly, poured into the mold after curing molding, and left to stand to remove bubbles. Then, heated at 60℃ for 1h to cure to obtain a SLMPD / PDMS composite layer.

[0061] Take silicone rubber E625 A and silicone rubber E625 B, mix evenly, pour into the mold, and stand to remove bubbles. Then, heat at 60°C for 1 h to make the silicone glue second curing molding, to obtain the piezoluminescence composite material, recorded as SG / SLMPD / PDMS / SG composite material.

[0062] Comparative example 1

[0063] The preparation of SLMPD / PDMS composite material, including the following steps:

[0064] According to the mass ratio 1:2:0.2, SLMPD, organosiloxane (SYLGARD 184 Silicone Elastomer Base) and silicone resin solution (SYLGARD 184 Silicone Elastomer Curing Agent) are weighed together 3.2g, mixed evenly, poured into the mold, and stood to remove bubbles. Heat at 60°C for 1 h to cure PMDS, to obtain SLMPD / PDMS composite material.

[0065] Figure 1 The powder XRD spectrum of SLMPD, from Figure 1 It can be seen that the product is pure phase Sr9LiMg(PO4)7, Dy 3+ Doping does not cause structural changes or introduce impurities.

[0066] Figure 2 The piezoluminescence spectrum of SLMPD / PDMS composite material. From Figure 2 It can be seen that SLMPD / PDMS composite material has Dy 3+ The emission peak of yellow light.

[0067] Figure 3 The piezoluminescence spectrum of SLMPD / PDMS composite material under different deformation. It can be seen that with the increase of deformation, the piezoluminescence intensity also increases. The maximum deformation can only be 100%, and the composite material will be broken when the deformation exceeds 100%.

[0068] Figure 4 The piezoluminescence spectrum of SG / SLMPD / PDMS / SG composite material under different deformation. From Figure 4 It can be seen that with the increase of deformation, the piezoluminescence intensity also increases. The maximum deformation is 180%.

[0069] Figure 5The fitting comparison diagram of the deformation and the photoluminescence intensity of SG / SLMPD / PDMS / SG composite and SLMPD / PDMS composite is shown in FIG. 6. It can be seen from the diagram that the deformation of SLMPD / PDMS composite can only reach 100%, while the deformation of SG / SLMPD / PDMS / SG composite can reach 180%. The slope of the fitting curve also increases from 146.16 of SLMPD / PDMS composite to 298.75 of SG / SLMPD / PDMS / SG composite. In summary, the preparation method effectively improves the flexibility and sensitivity of the traditional composite.

[0070] The above only describes the preferred embodiments of the present application, and it should be noted that those skilled in the art can make several improvements and refinements without departing from the principles of the present application, and these improvements and refinements should also be considered within the protection scope of the present application.

Claims

1. A mechanoluminescent composite material, characterized in that, The preparation method includes the following steps: After mixing silicone rubber E625 A and silicone rubber E625 B components, a first curing process is performed to obtain a silicone rubber layer. A SLMPD / PDMS composite material is fixed on the surface of an organosilicon rubber layer to form a SLMPD / PDMS composite layer; the SLMPD is Sr9LiMg(PO4)7:Dy 3+ ; After mixing silicone rubber E625 A and silicone rubber E625 B components, a second curing process is performed on the surface of the SLMPD / PDMS composite layer to obtain the mechanoluminescent composite material. The preparation method of the SLMPD / PDMS composite material is as follows: SLMPD, organosiloxane and curing agent are mixed and cured to obtain SLMPD / PDMS composite material; The mass ratio of SLMPD, organosiloxane, and curing agent is 0.8:1.5:0.13; The organosiloxane is SYLGARD 184 Silicone Elastomer Base; The mass ratio of the silicone rubber E625 A to the silicone rubber E625 B is 1:

1. The first curing and the second curing are independently cured at 60°C for 1 hour. The deformation of the mechanoluminescent composite material is 180%.

2. The application of the mechanoluminescent composite material of claim 1 in smart sensing, flexible electronic skin and wearable devices.

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