OPTICAL MEMBER WITH REDUCED LOW-MOLECULAR-WEIGHT SILOXANE CONTENT, AND METHOD FOR PRODUCING SAME

Abstract

The present invention provides: a highly transparent optical member which is formed from a silicone resin or a silicone rubber, and which has less mass change and excellent heat resistance without causing contact faults, or deterioration or contamination of the surface of other members due to adhesion to an electronic circuit or the surfaces of other members; and a production method for producing said optical member. According to the production method, the content of low-molecular-weight siloxanes D.sub.3-D.sub.20 in a optical member is reduced to an infinitesimal amount with use of a plurality of different low-molecular-weight siloxane removal steps.

Claims

1. An optical member formed from a silicone resin or a silicone rubber and transmitting or guiding light; wherein a total value of content of low-molecular-weight siloxanes D3-D20 is 100 ppm or less.

2. The optical member according to claim 1, wherein the total value of content of low-molecular-weight siloxanes D3-D20 of the optical member is 65 ppm or less.

3. The optical member according to claim 1, wherein the total value of content of low-molecular-weight siloxanes D3-D20 of the optical member is 50 ppm or less.

4. The optical member according to claim 1, wherein the total value of content of low-molecular-weight siloxanes D3-D20 of the optical member is 25 ppm or less.

5. The optical member according to claim 1, wherein the optical member has transmittance of 80% or more in the entire range of visible light wavelength region and near infrared wavelength region of 380 nm to 1,000 nm.

6. The optical member according to claim 1, wherein representative thickness of the optical member is 30 mm or less.

7. The optical member according to claim 1, wherein the optical member is an in-vehicle optical member.

8. The optical member according to claim 1, wherein the optical member has a shape having alignment part with another member.

9. The optical member according to claim 1, wherein the optical member does not contain a natural silica or a synthetic silica.

10. An optical member, wherein the optical member according to claim 1 is integrally molded or adhesively bonded after molding into one body with a material other than the silicone or another molded product.

11. A production method of producing the optical member according to claim 1, comprising: a low-molecular-weight siloxane removing step (A); and a low-molecular-weight siloxane removing step (B) being different from the low-molecular-weight siloxane removing step (A).

12. The production method of producing according to claim 11, wherein the low-molecular-weight siloxane removing step (A) is a step of reducing mainly low-molecular-weight siloxane D3-D10, wherein the low-molecular-weight siloxane removing step (B) is a step of reducing mainly low-molecular-weight siloxane D11-D20.

13. The production method of producing according to claim 12, wherein the low-molecular-weight siloxane removing step (A) is a heat treatment of the optical member, wherein the low-molecular-weight siloxane removing step (B) is immersing the optical member in an organic solvent to remove low-molecular-weight siloxane.

Description

BRIEF DESCRIPTION OF THE DRAWINGS

[0045] FIG. 1 is a graphic diagram of an experimental results shown in Table 1 according to the invention of the present application.

[0046] FIG. 2 is a graph showing transmittance according to the invention of the present application.

[0047] FIG. 3a is a drawing illustrating a representative thickness of an optical member according to the invention of the present application.

[0048] FIG. 3b is a drawing illustrating a representative thickness of an optical member according to the invention of the present application.

[0049] FIG. 3c is a drawing illustrating a representative thickness of an optical member according to the invention of the present application.

DESCRIPTION OF THE EMBODIMENTS

[0050] The optical member of the present invention is possible to reduce risk of contact faults, or of deterioration or contamination of the surfaces of other members due to adhesion to an electronic circuit incorporated with the optical member or to the surfaces of other members, and to reduce risk of mass change caused by volatilization of contained low-molecular-weight siloxane due to heating on the optical member, because the total value of content of low-molecular-weight siloxanes D.sub.3-D.sub.20 in the optical member formed from a silicone resin or a silicone rubber and transmits or guides light is 100 ppm or less, compared to cases where a total value of content of low-molecular-weight siloxanes D.sub.3-D.sub.20 is, for example, as large as 1,000 ppm. In the case of, preferably, the total value of content of low-molecular-weight siloxanes D.sub.3-D.sub.20 is 65 ppm or less, more preferably, the total value of content of low-molecular-weight siloxanes D.sub.3-D.sub.20 is 50 ppm or less, and even more preferably, the total value of content of low-molecular-weight siloxanes D.sub.3-D.sub.20 is 25 ppm or less, it is favorable as it leads to better result of reducing risk of contact faults, or deterioration or contamination of the surfaces of other members due to adhesion to the electronic circuit or the surfaces of other members, and reducing mass change caused by volatilization of low-molecular-weight siloxane in the optical member due to heating.

[0051] On the other hand, in the case of the total value of content of low-molecular-weight siloxanes D.sub.3-D.sub.20 of an optical member is large, for example 1,000 ppm, contained low-molecular-weight siloxane volatilizes and reduces the mass of the optical member and changes the product dimensions when the optical member which is formed from a silicone resin or a silicone rubber is heated by heat generated by lighting of an LED light source and the like located extremely close or temperature environment of the outside air, resulting in the loss of desired optical characteristics. Therefore, it is favorable to set the total value of content of low-molecular-weight siloxane D.sub.3-D.sub.20 to 100 ppm or less, preferably the total value of content of low-molecular-weight siloxane D.sub.3-D.sub.20 to 65 ppm or less, more preferably, the total value of content of low-molecular-weight siloxane D.sub.3-D.sub.20 to 50 ppm or less, and further more preferably, the total value of content of low-molecular-weight siloxane D.sub.3-D.sub.20 to 25 ppm or less, in which product dimension change due to volatility of low-molecular-weight siloxane is smaller. Thus, for example, even if the optical member is located extremely close to high-power LED light source, it is possible to maintain desired optical characteristics because product dimension change due to reduction of mass of the optical member caused by heating of the optical member by heat generated by lighting and volatility of low-molecular-weight siloxane can be prevented. If change in product dimensions due to mass reduction of the optical member is +/−2% or less, preferably +/−1% or less, it is possible to maintain desired optical characteristics of the optical member.

[0052] The optical member of the present invention does not have restriction in shape, and the shape can be adjusted according to desired function or characteristics of the optical member such as collection, diffusion and guide of light from a light source.

[0053] Further, it is preferable that the optical member of the present invention has a shape with alignment parts as it makes it easy to mount on other members. The light source in this case includes LED light source, LD light source, electroluminescence, xenon lamp, halogen lamp, sunlight and the like.

[0054] As for representative thickness of the optical member of the present invention, since low-molecular-weight siloxane removing step requires a long time, it is preferable that the representative thickness of the optical member of the present invention is 30 mm or less, preferably 20 mm or less, more preferably 10 mm or less, and further more preferably 5 mm or less in order to obtain product with industrial efficiency, in which the total value of content of low-molecular-weight siloxane can be 100 ppm or less with no requirement of long-time low-molecular-weight siloxane removing step.

[0055] The representative thickness refers to a thickness which represents the optical member, which is, for example, as shown in FIG. 3a to FIG. 3c, the longest side of the optical member, or if a circle is included such as a cylinder or a cone, D is the representative thickness if H>D, and H is the representative thickness if H<D, where the diameter is set to D and the height of the optical member such as cylinder or cone is set to H. Since it is easier to remove low-molecular-weight siloxane in a thin part than in a thick part, above values are used as an index to predict removal effect without depending on the shape considering that removal effect differs depending on the shape even if volume is the same. Taking up a rectangular parallelepiped of FIG. 3a as an example, the representative thickness of the rectangular parallelepiped is H where the longest side is set to D and the shortest side is set to height H. Also, using an example of a cylindrical shape of FIG. 3b, where its diameter is set to D when the circle is a perfect circle, otherwise, the diameter on the minor axis side is set to D and the height is set to H, if D is smaller, the representative thickness is D. And, if H is smaller than D, H is the representative thickness. Similarly in the case of a cone, if D is smaller than H, D is the representative thickness.

[0056] Further, in the case of a shape having a plurality of lenses on a rectangular parallelepiped as in FIG. 3c, where the longest side is set to D and heights of optical member are set to H and H′, if D>H>H′ is true then the representative thickness of the complicated shape is H. Even in shapes other than the shape examples shown in FIG. 3a to FIG. 3c, it is possible, from the viewpoint of penetration distance of the organic solvent, to predict the effect of removing low-molecular-weight siloxane and set the processing content properly by setting the representative thickness the smallest thickness when the entire object is considered to be a rough three-dimensional shape.

[0057] Hardness of the optical member of the present invention is not particularly restricted, and the silicone resin or the silicone rubber as base material can be selected according to the shape, use, and characteristics which are desired for the product. Shore D hardness measured by the method of JIS K 7215 (Testing Methods for Durometer Hardness of Plastics) or Shore A hardness measured by the method of JIS K 6253 (Rubber, vulcanized or thermoplastic—Determination of hardness) may be utilized, for example, Shore A hardness of 10 to 20 may be favorable if a flexible optical member is considered and its self-standing shape is taken into account. Shore A hardness of 20 to 70 may be favorable if an optical member having a certain degree of elasticity and a functionality of restoring force against an external force. The hardness can be adjusted in the range of Shore A hardness 70 to Shore D hardness 50 in order to prevent surface of the optical member from being damaged while maintaining elasticity. Preferably shore A hardness 75 to shore D hardness 30, more preferably shore A hardness 80 to shore D hardness 30 is favorable.

[0058] When the optical member of the present invention has a thickness of 2 mm, it is preferable to have 80% or more of transmittance in the entire range of visible light wavelength region and near infrared wavelength region of 380 nm to 1,000 nm even if required optical characteristic is low level and cost is to be prioritized such as light diffusion cover and light transmission cover, and 85% or more is preferable if both of cost and optical characteristic are to be achieved such as light guide member with short optical path length, and 90% or more is preferable if higher level of optical characteristic is required.

[0059] Inclusion or exclusion of a natural silica or a synthetic silica in the optical member of the present invention is selectable depending on required characteristics, and it is preferable not to add the natural silica or the synthetic silica if high transparency and transmission are required in the molded product. It is preferable to add the natural silica or the synthetic silica in case improved heat resistance or imparting light diffusivity from a light source is required, and amount thereof is adjustable according to desired functionality so that transmittance in the entire range of visible light wavelength region and near infrared wavelength region of 380 nm to 1,000 nm is 80% or more. For example, 0.01% to 0.5% by mass is preferable.

[0060] Further, it is not restricted to add additives such as antistatic agent, retarder, ultraviolet absorber and pigment in the optical member of the present invention as long as effects of the present invention are not impaired, and blending amount thereof can be adjusted according to desired functionality.

[0061] Materials of the optical member of the present invention is not particularly restricted as long as base material is silicone resin or silicone rubber, the base material can be a solid silicone resin or silicone rubber before curing, a semi-solid silicone resin or silicone rubber before curing, and a liquid silicone resin or silicone rubber before curing, and it is possible to select curing method of silicone to meet desired function of the optical member and the shape of the optical member, selectable from thermosetting silicone resin or silicone rubber, photosetting silicone resin or silicone rubber, and photosetting-thermosetting silicone resin or silicone rubber and the like or combination thereof. Among them, the liquid silicone resin or silicone rubber before curing is preferably used, and it is possible to mold even a complicated shape of the optical member.

[0062] Further, the liquid addition reaction curable silicone resin or silicone rubber before curing is more preferable as it can be molded into a complicated optical member shape and has less impurities generated during reaction than condensation curing silicone resin or silicone rubber, and an optical member with high transparency can be formed from it.

[0063] It is not particularly restricted as long as it is an addition reaction curable silicone resin or silicone rubber. Above all, thermosetting addition reaction curable silicone resin or silicone rubber is preferable as the optical member can be easily formed from. For example, a composition using an organopolysiloxane as base polymer and containing an organohydrogenpolysiloxane and a heavy metal catalyst such as platinum-based catalyst can be used.

[0064] Type and amount of the organohydrogenpolysiloxane and the catalyst may be appropriately determined taking the degree of cross-linking and curing rate into consideration, and a dimethylpolysiloxane or a dimethylsiloxane may be selected for base polymer if heat resistance functionality is required, and a methylphenylsiloxane copolymer may be selected for base polymer if higher refractive index functionality is required.

[0065] Molding method of the optical member of the present invention is not particularly restricted, and known molding methods can be used. For example, compression molding, injection molding, transfer molding, extrusion molding, calendar molding, coating molding, insert molding, molding by a 3D printer, and the like can be used.

[0066] The compression molding or the injection molding is preferable for a three-dimensional optical member based on optical design. Among them, the injection molding is preferable as it has less loss of base material and an optical member with complicated shape can be formed in fast molding cycle by using addition reaction of curable silicone resin or silicone rubber as base material being a liquid before curing.

[0067] Further, the optical member of the present invention may be a member in which the silicone resin or the silicone rubber as base material and a material other than silicone or other molded product are integrally molded or adhesively bonded after molding.

[0068] Light may be extracted efficiently and it is possible to selectively mold the optical member according to product design, for example, by combining with a member having light-shielding property or reflective property or composition thereof and another resin and the like by blending additive or the like to material or metal having light-shielding property or reflective property, and the silicone resin or the silicone rubber as base material, at a part other than where the light from a light source is necessary to transmit or to be guided. In such a case, integral molding is easily possible by performing insert molding. Here, materials other than the silicone include resin materials such as an epoxy resin and an acrylic resin, thermoplastics such as an engineering plastic and a super engineering plastic, thermosetting resins, optically excellent resins such as a cycloolefin polymer resin (COP) and a polyether sulfone resin (PES), metals such as aluminum, titanium, stainless steel, gold, silver and copper, glass and ceramics and the like can be used.

[0069] Further, in the above, the other molded product refers to a molded product which is molded in another step such as an optical member having a different shape.

[0070] Production method of the optical member according to the present invention is a production method comprising a low-molecular-weight siloxane removing step (A) and a low-molecular-weight siloxane removing step (B) which is different from the low-molecular-weight siloxane removing step (A), in which it is possible to obtain an optical member having the total value of content of low-molecular-weight siloxanes D.sub.3-D.sub.20 of 100 ppm or less by performing two or more types of low-molecular-weight siloxane removing steps on the low-molecular-weight siloxane and the low-molecular-weight siloxane removing steps may be performed by selecting and combining steps such as heat treatment of the molded optical member, heat treatment and immersion in an organic solvent in a vacuum or reduced pressure environment, cleaning with steam of an organic solvent and extraction of a critical fluid. Among them, it is preferable that the low-molecular-weight siloxane removing step (A) is heat treatment and the low-molecular-weight siloxane removing step (B) is immersion in an organic solvent, because the optical member of the present invention can be produced with high production efficiency in this way. In this case, low-molecular-weight siloxane can be removed more efficiently by performing a low-molecular-weight siloxane removing step by immersing in an organic solvent or the like after performing the heat treatment under reduced pressure environment or vacuum environment.

[0071] Further, during the step of removing the low-molecular-weight siloxane by immersing in the organic solvent, it is preferable to perform ultrasonic treatment or stirring and the like as well, so that low-molecular-weight siloxane can be removed more efficiently in a shorter treatment time.

[0072] The organic solvent used in the step of removing low-molecular-weight siloxane by immersing the molded optical member in the organic solvent is preferably an organic solvent having a solubility parameter (SP value) close to that of the silicone which is the base material of the optical member, and organic solvents having a solubility parameter (SP value) of 6 to 9 are particularly preferable. For example, n-butane, n-pentane, n-hexane, 1-bromopropane, 1-bromobutane and the like may be mentioned.

[0073] The total value of content thereof can be 50 ppm or less, or even 25 ppm or less by adjusting treatment time and temperature.

[0074] Further, the production method of the optical member according to the present invention may include a drying step of drying the organic solvent in the optical member as a post-step of the low-molecular-weight siloxane removing step of immersing in the organic solvent, and the drying temperature is not particularly restricted.

[0075] The optical member according to the present invention effectively prevents generation of volatile component which causes contact faults, or deterioration or contamination of the surfaces of other members by adhesion to the electronic circuit and the surfaces of other members, even used in high temperature places, because the content of low-molecular-weight siloxanes but relatively large molecule in conventional low-molecular-weight siloxanes of up to D.sub.20 is such an unbelievably low content.

[0076] Further, the optical member according to the present invention has an exceptionally advantageous effect that volatile component is significantly low as a member requiring thickness, since the content of low-molecular-weight siloxane is remarkably low even if it is much thicker than a conventional member.

[0077] The thicker the member is, the more difficult it is to reduce low-molecular-weight siloxane content conventionally, however, as can be seen from embodiments described below, the optical member according to the present invention is characterized in that, even if thickness value is the same, the content of low-molecular-weight siloxane is significantly reduced to the level unbelievable in conventional members.

[0078] Further, according to the method of the present invention, it is possible to perform processes of reducing the content much more than conventional method in shorter time and in greater volume.

EMBODIMENTS

[0079] In the embodiments, heating temperature is preferably 130° C. or higher, and solvent extraction time for gas chromatography measurement is preferably selected in the range of 1 hour or more and 20 hours or less according to material properties.

[0080] In addition, in order to evaluate the stability of the shape of the optical member against heating, shape change rate was judged to be “success” if shape change rate is +/−1% and otherwise to be “fail” by a test at 120° C. for 500 hours.

Embodiment 1

[0081] A silicone optical member with 70 mm square and representative thickness of 0.5 mm was molded, and the optical member was heat-treated in a heating oven for 3 to 6 hours, and then the optical member was immersed in 2 liters of 1-bromopropane in a beaker stirring for 6 to 12 hours. Then, the optical member was removed from 1-bromopropane, and the optical member was dried. In order to measure the contained low-molecular-weight siloxanes D.sub.3-D.sub.20, the dried optical member was cut into 1 to 2 mm square, 0.5 g thereof was sampled and was immersed in 5 ml of special grade chromatographic hexane for 16 hours, then low-molecular-weight siloxanes D.sub.3-D.sub.20 contained in the optical member was eluted.

[0082] Eluted content was quantified by gas chromatography, and the content of low-molecular-weight siloxanes D.sub.3-D.sub.20 contained in the optical member was calculated.

Embodiment 2

[0083] Processes and gas chromatography were performed in the same manner as in Embodiment 1 except that a silicone optical member with 70 mm square and representative thickness of 2.0 mm was molded, low-molecular-weight siloxane contained in the optical member was quantified, and the content of low-molecular-weight siloxanes D.sub.3-D.sub.20 contained in the optical member was calculated.

Embodiment 3

[0084] Processes and gas chromatography were performed in the same manner as in Embodiment 1 except that a silicone optical member with 70 mm square and representative thickness of 5.0 mm was molded, low-molecular-weight siloxane contained in the optical member was quantified, and the content of low-molecular-weight siloxanes D.sub.3-D.sub.20 contained in the optical member was calculated.

Embodiment 4

[0085] Processes and gas chromatography were performed in the same manner as in Embodiment 1 except that a silicone optical member with 70 mm square and representative thickness of 10 mm was molded, low-molecular-weight siloxane contained in the optical member was quantified, and the content of low-molecular-weight siloxanes D.sub.3-D.sub.20 contained in the optical member was calculated.

Embodiment 5

[0086] Processes and gas chromatography were performed in the same manner as in Embodiment 1 except that a silicone optical member with 70 mm square and representative thickness of 20 mm was molded, low-molecular-weight siloxane contained in the optical member was quantified, and the content of low-molecular-weight siloxanes D.sub.3-D.sub.20 contained in the optical member was calculated.

Embodiment 6

[0087] Processes and gas chromatography were performed in the same manner as in Embodiment 1 except that a silicone optical member with 70 mm square and representative thickness of 30 mm was molded, low-molecular-weight siloxane contained in the optical member was quantified, and the content of low-molecular-weight siloxanes D.sub.3-D.sub.20 contained in the optical member was calculated.

Comparative Example 1

[0088] Processes and gas chromatography were performed in the same manner as in Embodiment 1 except that a silicone optical member with 70 mm square and representative thickness of 40 mm was molded, low-molecular-weight siloxane contained in the optical member was quantified, and the content of low-molecular-weight siloxanes D.sub.3-D.sub.20 contained in the optical member was calculated.

Comparative Example 2

[0089] Processes and gas chromatography were performed in the same manner as in Embodiment 1 except that a silicone optical member with 70 mm square and representative thickness of 50 mm was molded, low-molecular-weight siloxane contained in the optical member was quantified, and the content of low-molecular-weight siloxanes D.sub.3-D.sub.20 contained in the optical member was calculated.

Comparative Example 3

[0090] A silicone optical member with 70 mm square and representative thickness of 0.5 mm was molded, the process for removing low-molecular-weight siloxane as in Embodiment 1 was not performed, dried optical member was cut into 1 to 2 mm square to measure low-molecular-weight siloxane D.sub.3-D.sub.20 contained in the optical member, 0.5 g thereof was sampled and was immersed in 5 ml of special grade chromatographic hexane for 16 hours, then low-molecular-weight siloxanes D.sub.3-D.sub.20 contained in the optical member was eluted. This was quantified by gas chromatography, and the content of low-molecular-weight siloxanes D.sub.3-D.sub.20 contained in the optical member was calculated.

Comparative Example 4

[0091] The process was performed in the same manner, except that a silicone optical member with 70 mm square and representative thickness of 2.0 mm was molded, as in Comparative example 3, i.e. removing low-molecular-weight siloxane was not performed, and gas chromatography was performed to quantify low-molecular-weight siloxane contained in the optical member, and the content of low-molecular-weight siloxanes D.sub.3-D.sub.20 contained in the optical member was calculated.

Comparative Example 5

[0092] The process for removing low-molecular-weight siloxane was not performed as the same manner as in Comparative example 3 except that a silicone optical member with 70 mm square and representative thickness of 5.0 mm was molded, gas chromatography was performed to quantify low-molecular-weight siloxane contained in the optical member, and the content of low-molecular-weight siloxanes D.sub.3-D.sub.20 contained in the optical member was calculated.

Comparative Example 6

[0093] The process for removing low-molecular-weight siloxane was not performed as in the same manner as in Comparative example 3 except that a silicone optical member with 70 mm square and representative thickness of 10 mm was molded, gas chromatography was performed to quantify low-molecular-weight siloxane contained in the optical member, and the content of low-molecular-weight siloxanes D.sub.3-D.sub.20 contained in the optical member was calculated.

Comparative Example 7

[0094] The process for removing low-molecular-weight siloxane was not performed as in the same manner as in Comparative example 3 except that a silicone optical member with 70 mm square and representative thickness of 20 mm was molded, gas chromatography was performed to quantify low-molecular-weight siloxane contained in the optical member, and the content of low-molecular-weight siloxanes D.sub.3-D.sub.20 contained in the optical member was calculated.

Comparative Example 8

[0095] The process for removing low-molecular-weight siloxane was not performed as in the same manner as in Comparative example 3 except that a silicone optical member with 70 mm square and representative thickness of 30 mm was molded, gas chromatography was performed to quantify low-molecular-weight siloxane contained in the optical member, and the content of low-molecular-weight siloxanes D.sub.3-D.sub.20 contained in the optical member was calculated.

Comparative Example 9

[0096] The process for removing low-molecular-weight siloxane was not performed as in the same manner as in Comparative example 3 except that a silicone optical member with 70 mm square and representative thickness of 40 mm was molded, gas chromatography was performed to quantify low-molecular-weight siloxane contained in the optical member, and the content of low-molecular-weight siloxanes D.sub.3-D.sub.20 contained in the optical member was calculated.

Comparative Example 10

[0097] The process for removing low-molecular-weight siloxane was not performed as in the same manner as in Comparative example 3 except that a silicone optical member with 70 mm square and representative thickness of 50 mm was molded, gas chromatography was performed to quantify low-molecular-weight siloxane contained in the optical member, and the content of low-molecular-weight siloxanes D.sub.3-D.sub.20 contained in the optical member was calculated.

Comparative Example 11

[0098] A silicone optical member with 70 mm square and representative thickness of 0.5 mm was molded, only a heat treatment for 3 to 6 hours to remove low-molecular-weight siloxane was performed, dried optical member was cut into 1 to 2 mm square to measure low-molecular-weight siloxane D.sub.3-D.sub.20 contained in the optical member, 0.5 g thereof was sampled and was immersed in 5 ml of special grade chromatographic hexane for 16 hours, then low-molecular-weight siloxanes D.sub.3-D.sub.20 contained in the optical member was eluted. This was quantified by gas chromatography, and the content of low-molecular-weight siloxanes D.sub.3-D.sub.20 contained in the optical member was calculated.

Comparative Example 12

[0099] Only a heat treatment for 3 to 6 hours to remove low-molecular-weight siloxane was performed as in the same manner as in Comparative example 11 except that a silicone optical member with 70 mm square and representative thickness of 2.0 mm was molded, gas chromatography was performed to quantify low-molecular-weight siloxane contained in the optical member, and the content of low-molecular-weight siloxanes D.sub.3-D.sub.20 contained in the optical member was calculated.

Comparative Example 13

[0100] Only a heat treatment for 3 to 6 hours to remove low-molecular-weight siloxane was performed as in the same manner as in Comparative example 11 except that a silicone optical member with 70 mm square and representative thickness of 5.0 mm was molded, gas chromatography was performed to quantify low-molecular-weight siloxane contained in the optical member, and the content of low-molecular-weight siloxanes D.sub.3-D.sub.20 contained in the optical member was calculated.

Comparative Example 14

[0101] Only a heat treatment for 3 to 6 hours to remove low-molecular-weight siloxane was performed as in the same manner as in Comparative example 11 except that a silicone optical member with 70 mm square and representative thickness of 10 mm was molded, gas chromatography was performed to quantify low-molecular-weight siloxane contained in the optical member, and the content of low-molecular-weight siloxanes D.sub.3-D.sub.20 contained in the optical member was calculated.

Comparative Example 15

[0102] Only a heat treatment for 3 to 6 hours to remove low-molecular-weight siloxane was performed as in the same manner as in Comparative example 11 except that a silicone optical member with 70 mm square and representative thickness of 20 mm was molded, gas chromatography was performed to quantify low-molecular-weight siloxane contained in the optical member, and the content of low-molecular-weight siloxanes D.sub.3-D.sub.20 contained in the optical member was calculated.

Comparative Example 16

[0103] Only a heat treatment for 3 to 6 hours to remove low-molecular-weight siloxane was performed as in the same manner as in Comparative example 11 except that a silicone optical member with 70 mm square and representative thickness of 30 mm was molded, gas chromatography was performed to quantify low-molecular-weight siloxane contained in the optical member, and the content of low-molecular-weight siloxanes D.sub.3-D.sub.20 contained in the optical member was calculated.

Comparative Example 17

[0104] Only a heat treatment for 3 to 6 hours to remove low-molecular-weight siloxane was performed as in the same manner as in Comparative example 11 except that a silicone optical member with 70 mm square and representative thickness of 40 mm was molded, gas chromatography was performed to quantify low-molecular-weight siloxane contained in the optical member, and the content of low-molecular-weight siloxanes D.sub.3-D.sub.20 contained in the optical member was calculated.

Comparative Example 18

[0105] Only a heat treatment for 3 to 6 hours to remove low-molecular-weight siloxane was performed as in the same manner as in Comparative example 11 except that a silicone optical member with 70 mm square and representative thickness of 50 mm was molded, gas chromatography was performed to quantify low-molecular-weight siloxane contained in the optical member, and the content of low-molecular-weight siloxanes D.sub.3-D.sub.20 contained in the optical member was calculated.

Comparative Example 19

[0106] A silicone optical member with 70 mm square and representative thickness of 0.5 mm was molded, and the optical member was immersed in 2 liters of 1-bromopropane in a beaker stirring for 20 to 30 hours. Then, the optical member was removed from 1-bromopropane, and the optical member was dried. In order to measure contained low-molecular-weight siloxanes D.sub.3-D.sub.20, the dried optical member was cut into 1 to 2 mm square, 0.5 g thereof was sampled and was immersed in 5 ml of special grade chromatographic hexane for 16 hours, then low-molecular-weight siloxanes D.sub.3-D.sub.20 contained in the optical member was eluted. This was quantified by gas chromatography, and the content of low-molecular-weight siloxanes D.sub.3-D.sub.20 contained in the optical member was calculated.

Comparative Example 20

[0107] Only an immersion treatment in organic solvent for 20 to 30 hours to remove low-molecular-weight siloxane was performed as in the same manner as in Comparative example 19 except that a silicone optical member with 70 mm square and representative thickness of 2.0 mm was molded, gas chromatography was performed to quantify low-molecular-weight siloxane contained in the optical member, and the content of low-molecular-weight siloxanes D.sub.3-D.sub.20 contained in the optical member was calculated.

Comparative Example 21

[0108] Only an immersion treatment in organic solvent for 20 to 30 hours to remove low-molecular-weight siloxane was performed as in the same manner as in Comparative example 19 except that a silicone optical member with 70 mm square and representative thickness of 5.0 mm was molded, gas chromatography was performed to quantify low-molecular-weight siloxane contained in the optical member, and the content of low-molecular-weight siloxanes D.sub.3-D.sub.20 contained in the optical member was calculated.

Comparative Example 22

[0109] Only an immersion treatment in organic solvent for 20 to 30 hours to remove low-molecular-weight siloxane was performed as in the same manner as in Comparative example 19 except that a silicone optical member with 70 mm square and representative thickness of 10 mm was molded, gas chromatography was performed to quantify low-molecular-weight siloxane contained in the optical member, and the content of low-molecular-weight siloxanes D.sub.3-D.sub.20 contained in the optical member was calculated.

Comparative Example 23

[0110] Only an immersion treatment in organic solvent for 20 to 30 hours to remove low-molecular-weight siloxane was performed as in the same manner as in Comparative example 19 except that a silicone optical member with 70 mm square and representative thickness of 20 mm was molded, gas chromatography was performed to quantify low-molecular-weight siloxane contained in the optical member, and the content of low-molecular-weight siloxanes D.sub.3-D.sub.20 contained in the optical member was calculated.

Comparative Example 24

[0111] Only an immersion treatment in organic solvent for 20 to 30 hours to remove low-molecular-weight siloxane was performed as in the same manner as in Comparative example 19 except that a silicone optical member with 70 mm square and representative thickness of 30 mm was molded, gas chromatography was performed to quantify low-molecular-weight siloxane contained in the optical member, and the content of low-molecular-weight siloxanes D.sub.3-D.sub.20 contained in the optical member was calculated.

Comparative Example 25

[0112] Only an immersion treatment in organic solvent for 20 to 30 hours to remove low-molecular-weight siloxane was performed as in the same manner as in Comparative example 19 except that a silicone optical member with 70 mm square and representative thickness of 40 mm was molded, gas chromatography was performed to quantify low-molecular-weight siloxane contained in the optical member, and the content of low-molecular-weight siloxanes D.sub.3-D.sub.20 contained in the optical member was calculated.

Comparative Example 26

[0113] Only an immersion treatment in organic solvent for 20 to 30 hours to remove low-molecular-weight siloxane was performed as in the same manner as in Comparative example 19 except that a silicone optical member with 70 mm square and representative thickness of 50 mm was molded, gas chromatography was performed to quantify low-molecular-weight siloxane contained in the optical member, and the content of low-molecular-weight siloxanes D.sub.3-D.sub.20 contained in the optical member was calculated.

[0114] Table 1 below shows results of above embodiments and comparative examples.

TABLE-US-00001 Low-molecular-weight Thickness Low-molecular-weight siloxanes D3-D20 content Determination of (mm) siloxane removing step (ppm) shape change rate Embodiment 1 0.5 Heat treatment and 10 ◯ Embodiment 2 2.0 Organic solvent 10 ◯ Embodiment 3 5.0 immersion treatment 23 ◯ Embodiment 4 10 46 ◯ Embodiment 5 20 63 ◯ Embodiment 6 30 94 ◯ Comparative example 1 40 161 X Comparative example 2 50 285 X Comparative example 3 0.5 No treatment 470 X Comparative example 4 2.0 473 X Comparative example 5 5.0 482 X Comparative example 6 10 485 X Comparative example 7 20 484 X Comparative example 8 30 479 X Comparative example 9 40 466 X Comparative example 10 50 489 X Comparative example 11 0.5 Heat treatment only 267 X Comparative example 12 2.0 285 X Comparative example 13 5.0 298 X Comparative example 14 10 303 X Comparative example 15 20 310 X Comparative example 16 30 357 X Comparative example 17 40 430 X Comparative example 18 50 444 X Comparative example 19 0.5 Organic solvent 12 ◯ Comparative example 20 2.0 immersion treatment only 17 ◯ Comparative example 21 5.0 65 ◯ Comparative example 22 10 123 X Comparative example 23 20 176 X Comparative example 24 30 288 X Comparative example 25 40 376 X Comparative example 26 50 398 X

[0115] From the results in Table 1, in embodiments 1 to 6 in which heat treatment and immersion treatment in organic solvent were performed, since the content of low-molecular-weight siloxanes D.sub.3-D.sub.20 contained in the optical member is infinitesimal amount, it is possible to reduce risk of contact faults, or deterioration or contamination of the surfaces of other members due to adhesion to the electronic circuit incorporated with the optical member or surfaces of other members, mass change caused by volatilization of contained low-molecular-weight siloxane due to heating on the optical member is small, in which shape change rate is +/−1%. Comparative examples 19 to 21 also show the amount of low-molecular-weight siloxanes D.sub.3-D.sub.20 being infinitesimal amount, but an immersion treatment in organic solvent needs to be performed for a longer time than in embodiments 1 to 6, and in addition, the content is higher. According to the present invention, it is possible to remove low-molecular-weight siloxanes D.sub.3-D.sub.20 in a shorter time, to meet a market demand for further reduction of the content of low-molecular-weight siloxanes D.sub.3-D.sub.20, and to provide an optical member which is formed from a silicone resin or a silicone rubber in which precise optical design is required.