Isolating layer material formula

Abstract

The invention relates to an isolating layer material formula, and belongs to the technical field of biosensor manufacturing, according to the scheme, 118-08 type epoxy resin is adopted as a base material, a phthalocyanine blue BGS coloring agent with a specific proportion is added, so that the base material is blue, and an organic silicon flatting agent BYK-333 and a defoaming agent BYK-055 form a complete system. The key of the technical means is that the viscosity of the material is controlled to be 3000-5000 cPs, and a curing process of 80-100 DEG C / 10-30 minutes is adopted to form an isolating layer with the thickness of 20-50 microns. The material has no swelling or exudate after being in contact with hemolytic blood at 37 DEG C for 24 hours, the resistance change is less than or equal to 1% when the material is in contact with a system solution, and excellent biological stability and electrical reliability are shown. Meanwhile, the electrode material is well compatible with a screen-printed electrode material, is suitable for large-scale production, and provides a high-performance insulation protection solution for a biosensor.

Description

Technical Field

[0001] This invention relates to the field of biosensor technology, specifically to the formulation of isolation layer materials. Background Technology

[0002] In the manufacture of biosensors, especially blood detection sensors, the insulating layer is a crucial functional layer for achieving insulation between electrodes, defining the reaction area, and protecting the internal conductive path. Its performance directly affects the sensor's accuracy, stability, and lifespan. Currently, commonly used polymer insulating materials (such as certain polyimides or general-purpose epoxy resins) are prone to swelling and the precipitation of trace components when in prolonged contact with complex biological samples such as blood and serum. This physical deformation or chemical leaching not only alters the sensor's physical structure, causing volume drift in the detection area, but may also contaminate the sample or interfere with the electrochemical reactions on the electrode surface, ultimately leading to signal distortion, decreased accuracy, and even premature sensor failure. Furthermore, the adaptability of traditional materials in screen printing processes, interfacial compatibility with various electrode materials, and batch consistency in large-scale production still present numerous challenges, hindering the industrialization of high-performance, high-reliability biosensors.

[0003] With the widespread adoption of point-of-care testing (POCT) technology, higher demands are being placed on the robustness of biosensors in complex operating environments. For example, sensors need to maintain extremely stable insulation resistance throughout their operating temperature range and lifespan; any minute change in resistance can be amplified into significant measurement errors. Existing material formulations and processes often struggle to achieve an optimal balance between biocompatibility, electrical stability, process suitability, and cost control. Therefore, the industry urgently needs to develop a novel insulating layer material that not only withstands the corrosion of biological fluids and maintains long-term dimensional and chemical stability, but also exhibits excellent electrical inertness and is perfectly compatible with modern high-speed precision manufacturing processes, thus providing a reliable foundation for next-generation high-precision, long-life biosensors. Summary of the Invention

[0004] To address the problems of the prior art, this invention provides a formulation for an isolation layer material.

[0005] To solve the above-mentioned technical problems, the present invention is achieved through the following technical solution: Firstly, the isolation layer material formulation, wherein the isolation layer material is composed of 118-08 type epoxy resin and phthalocyanine blue BGS colorant, wherein the material does not swell or exudate after contacting a hemolyzed blood sample at 37°C for 24 hours, and the resistance change is ≤1% when in contact with the system solution.

[0006] In one specific embodiment of the first aspect, the insulating layer material is a 2k-epoxy resin system, which has solvent resistance, chemical corrosion resistance, and compatibility with screen-printed electrode materials and conductive path materials.

[0007] In one specific embodiment of the first aspect, the isolation layer material is a blue marking material, the color component of which is Phthalocyanine Blue BGS, and the content is 0.5%-1.5% of the total resin.

[0008] In one specific embodiment of the first aspect, the isolation layer material further comprises a leveling agent, said leveling agent being an organosilicon leveling agent BYK-333, added in an amount of 0.1%-0.5% of the total resin.

[0009] In one specific embodiment of the first aspect, the isolation layer material further comprises a defoamer, said defoamer being organosilicon defoamer BYK-055, added at an amount of 0.05%-0.2% of the total resin.

[0010] In one specific embodiment of the first aspect, the viscosity of the isolation layer material is 3000-5000 cPs (25°C), suitable for screen printing processes.

[0011] In one specific embodiment of the first aspect, the curing conditions of the isolation layer material after screen printing are: temperature 80-100°C, time 10-30 minutes;

[0012] The thickness of the isolation layer formed after curing is 20-50μm.

[0013] In one specific embodiment of the first aspect, the isolation layer material further comprises a dispersant, wherein the dispersant is a polymeric dispersant BYK-163, and the amount added is 0.1%-0.3% of the total amount of resin.

[0014] Secondly, a biosensor isolation layer is prepared from an isolation layer material formulation.

[0015] Thirdly, a biosensor comprising a biosensor isolation layer.

[0016] The beneficial effects of this invention are as follows:

[0017] 1. By employing a specific 118-08 type epoxy resin system and optimizing the formulation and preparation process of components such as pigments, leveling agents, and defoamers, significant improvements in material performance were achieved. Its beneficial effects are primarily reflected in its excellent biological stability and electrical reliability: after contact with hemolyzed blood samples at 37°C for up to 24 hours, the material exhibited no swelling or exudate, ensuring long-term stability under harsh biological environments; simultaneously, its resistance change upon contact with the system solution was strictly controlled within an extremely low range of ≤1%, with a volume resistivity as high as 10⁻⁶. 15 The Ω·cm provides a stable and precise electrical working environment for biosensors, directly ensuring the accuracy and reliability of detection results.

[0018] Secondly, this solution offers significant advantages in terms of process applicability, industrialization prospects, and overall benefits. The material possesses a suitable viscosity of 3000-5000 cPs (25℃), making it highly compatible with screen printing processes. Combined with optimized curing conditions, it can achieve a production efficiency of up to 1200 pieces / hour and a yield rate exceeding 98.5%, demonstrating excellent batch consistency and large-scale production capabilities. Furthermore, the material exhibits good compatibility with all functional layers of the sensor (such as conductive paths, electrodes, and enzyme layers), with no adverse interface reactions. The reduction in both material and maintenance costs results in an overall cost reduction of approximately 18% compared to traditional solutions. Clinical trials have shown that sensors using this isolation layer exhibit a 60% reduction in operational error rate and a user satisfaction rate as high as 95%, fully demonstrating its high reliability and practical value in real-world applications. Detailed Implementation

[0019] The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0020] Formulation of isolation layer material.

[0021] Example 1: Basic Formulation Research

[0022] This embodiment details the basic formulation and preparation process of the isolation layer material.

[0023] 1. Raw material preparation

[0024] 1.1 Main Resin System

[0025] Epoxy resin type 118-08: 100 parts by weight

[0026] This resin has the following properties:

[0027] Viscosity: 4500 cPs (25℃)

[0028] Solid content: 65%

[0029] Epoxy equivalent: 450-500

[0030] Color: Pale yellow transparent liquid

[0031] 1.2 Shading System

[0032] Phthalocyanine Blue BGS: 0.8 parts by weight

[0033] Pigment properties:

[0034] Hue: β-phthalocyanine blue

[0035] Particle size: 0.1-0.5μm

[0036] Heat resistance: 300℃

[0037] Migration resistance: Level 5

[0038] 1.3 Additive System

[0039] Leveling agent: Organosilicon leveling agent BYK-333, 0.3 parts by weight

[0040] Defoamer: Organosilicon defoamer BYK-055, 0.1 parts by weight

[0041] Dispersant: Polymer dispersant BYK-163, 0.2 parts by weight

[0042] 2. Preparation process

[0043] 2.1 Pre-dispersion stage

[0044] Add type 118-08 epoxy resin to a high-speed dispersion kettle, control the temperature at 25±2℃, and stir at 200 rpm. Add the dispersant and phthalocyanine blue BGS pigment in sequence, gradually increase the stirring speed to 1000 rpm, and continue dispersing for 30 minutes.

[0045] 2.2 Fine Grinding Stage

[0046] The pre-dispersed material is transferred to a three-roll mill for fine grinding. The grinding parameters are as follows:

[0047] Roller gap: 10μm for primary roller, 5μm for secondary roller.

[0048] Roller speeds: slow roller 15 rpm, medium roller 45 rpm, fast roller 135 rpm

[0049] Grinding times: 3 times

[0050] Temperature control: ≤40℃

[0051] 2.3 Additives Addition Stage

[0052] Return the ground material to the dispersion vessel, and add the leveling agent and defoamer sequentially under low-speed stirring (300 rpm). Stir for 15 minutes after each addition to ensure thorough mixing.

[0053] 2.4 Filter Packaging

[0054] The final product is filtered through a 400-mesh filter to remove any impurities and incompletely dispersed pigment aggregates. The product is then packaged in a sealed container and stored at 15-25°C.

[0055] 3. Quality Inspection

[0056] The following quality tests were performed on the prepared isolation layer material:

[0057] 3.1 Physical performance testing

[0058] Viscosity: Measured using a Brookfield viscometer, controlled within 4500±500 cPs (25℃).

[0059] Fineness: Measured using a scraper fineness gauge, ≤10μm

[0060] Color: Measured using a colorimeter, ΔE ≤ 1.0

[0061] 3.2 Storage stability test

[0062] The samples were aged at 40℃ for 30 days, and the following indicators were tested:

[0063] Viscosity change rate: ≤10%

[0064] Pigment settling properties: No hard sedimentation.

[0065] Performance: No change

[0066] Example 2: Formula Optimization Study

[0067] This embodiment systematically studies the influence of the dosage of each component on the material properties and determines the optimal formulation range.

[0068] 1. Resin system optimization

[0069] With other components kept constant, the effect of different batches of type 118-08 epoxy resin on its properties was investigated:

[0070] Batch A: Viscosity 4200 cPs, Epoxy Equivalent 480

[0071] Batch B: Viscosity 4600 cPs, epoxy equivalent 470

[0072] Batch C: Viscosity 4400 cPs, Epoxy Equivalent 490

[0073] Test results show that batch B has the best overall performance, exhibiting better leveling and pattern clarity during screen printing.

[0074] 2. Optimization of pigment usage

[0075] Investigating the effect of phthalocyanine blue (BGS) dosage on color depth and performance:

[0076] 0.5 parts by weight: Light in color, with average operability.

[0077] 0.8 parts by weight: Moderate color, good operability.

[0078] 1.2 parts by weight: Too dark a color will affect the depth of UV curing.

[0079] 1.5 parts by weight: The color is too dark and the viscosity has increased significantly.

[0080] The optimal dosage range was finally determined to be 0.8-1.0 parts by weight.

[0081] 3. Optimization of leveling agent dosage

[0082] Investigating the effect of BYK-333 leveling agent dosage on film quality:

[0083] 0.1 parts by weight: Insufficient leveling effect, resulting in orange peel effect.

[0084] 0.3 parts by weight: Good leveling effect, smooth film layer.

[0085] 0.5 parts by weight: Excellent leveling effect, but pinholes appear.

[0086] 4. Optimization of defoamer dosage

[0087] Investigating the effect of BYK-055 defoamer dosage on bubble formation:

[0088] 0.05 parts by weight: Defoaming effect is average, with some tiny bubbles still remaining.

[0089] 0.1 parts by weight: Good defoaming effect, no visible bubbles.

[0090] 0.2 parts by weight: Excellent defoaming effect, but affects leveling properties.

[0091] Example 3: Coating Process Study

[0092] This embodiment studies in detail the coating process parameters of the isolation layer material.

[0093] 1. Optimization of screen printing process

[0094] 1.1 Mesh Parameters: Mesh Material: Stainless Steel; Mesh Count: 350 Mesh; Wire Diameter: 28μm

[0095] Aperture: 45μm

[0096] Film thickness: 15μm

[0097] 1.2 Printing parameters: Squeegee angle: 75°

[0098] Printing speed: 100mm / s

[0099] De-grid speed: 5mm / s

[0100] Printing pressure: 0.3MPa

[0101] 1.3 Ambient temperature control: 23±2℃

[0102] Humidity: 50±5%RH

[0103] Cleanliness level: Class 10,000

[0104] 2. Curing process research

[0105] 2.1 Curing Temperature Optimization

[0106] Investigating the effect of different curing temperatures on film properties:

[0107] 80℃: Incomplete curing, poor adhesion.

[0108] 90℃: Good curing and optimal performance.

[0109] 100℃: Completely cured, but the color changes slightly.

[0110] 110℃: Over-curing increases the brittleness of the film layer.

[0111] 2.2 Curing Time Optimization

[0112] Curing time was studied at 90℃:

[0113] 10 minutes: Insufficient curing

[0114] 20 minutes: Complete curing

[0115] 30 minutes: Performance is comparable, but energy consumption increases.

[0116] 2.3 Temperature rise program optimization

[0117] A stepped heating program is used:

[0118] Phase 1: 25℃→60℃, time 5 minutes

[0119] Second stage: 60℃→90℃, time 10 minutes

[0120] Third stage: Maintain a constant temperature of 90℃ for 20 minutes.

[0121] Fourth stage: Allow to cool naturally to room temperature

[0122] Example 4: Performance Testing and Verification

[0123] This embodiment verifies the various performance indicators of the isolation layer material through system testing.

[0124] 1. Biological corrosion resistance test

[0125] 1.1 Hemolysis Blood Test

[0126] Prepare hemolyzed blood samples by immersing the isolation layer sample at 37°C for 24 hours and observing the following indicators:

[0127] Appearance changes: no swelling, no exudation; weight change: ≤0.1%.

[0128] Dimensional variation: ≤0.05%

[0129] 1.2 Long-term immersion test

[0130] The sample was immersed in physiological saline at 37℃ for 30 days, and the weight change rate was tested to be ≤0.3%.

[0131] Tensile strength retention: ≥95%

[0132] Appearance: No change

[0133] 2. Electrical performance testing

[0134] 2.1 Resistance Stability Test

[0135] Test the resistance change under the following conditions:

[0136] After immersion in the system solution for 24 hours: resistance change ≤1%.

[0137] Temperature cycling test (-20℃~60℃): resistance change ≤2%; Damp heat test (40℃, 93%RH): resistance change ≤1.5% 2.2 Insulation performance test

[0138] Volume resistivity: ≥10 15 Ω·cm

[0139] Surface resistivity: ≥10 14 Ω

[0140] Dielectric strength: ≥100kV / mm

[0141] 3. Mechanical performance testing

[0142] 3.1 Adhesion Test

[0143] Adhesion was tested using the cross-cut adhesion test.

[0144] Test standard: ASTM D3359

[0145] Result: Grade 5B (Best Grade)

[0146] Peel strength: ≥4.5 N / cm

[0147] 3.2 Hardness Test: Pencil hardness: ≥4H

[0148] Shore hardness: ≥85D

[0149] 3.3 Abrasion resistance test standard: ASTM D4060

[0150] Results: Weight loss ≤2mg / 1000 times

[0151] Example 5: Compatibility Study with Electrode Materials

[0152] This embodiment studies the compatibility between the isolation layer material and the various functional layers of the sensor.

[0153] 1. Compatibility with conductive paths

[0154] 1.1 Conductive path of silver-palladium alloy (EL44-040)

[0155] Adhesion: Grade 5B; Interfacial resistance: No change.

[0156] Long-term stability: No degradation after 1000 hours

[0157] 1.2 Contact Resistance Test

[0158] Testing contact resistance changes under high temperature and high humidity conditions:

[0159] Initial contact resistance: ≤0.1Ω; after 1000 hours: ≤0.12Ω

[0160] Change rate: ≤20%

[0161] 2. Compatibility with electrode materials

[0162] 2.1 Platinum working electrode (E1192)

[0163] Interface characteristics: No response

[0164] Electrochemical performance: No effect

[0165] Long-term stability: Good

[0166] 2.2 Silver / Silver Chloride Reference Electrode (5876)

[0167] Chemical stability: Non-corrosive

[0168] Potential stability: Drift ≤ 2mV

[0169] Service life: No impact

[0170] 3. Compatibility with enzyme layers

[0171] 3.1 Interface Features

[0172] No penetration phenomenon

[0173] No chemical reaction

[0174] Good adhesion

[0175] 3.2 Effect on enzyme activity: Glucose oxidase activity: No effect; Long-term stability: No change.

[0176] Example 6: Environmental Impact Study

[0177] This embodiment studies the performance of the isolation layer material under different environmental conditions.

[0178] 1. Study on the effects of temperature

[0179] Material properties were tested within a temperature range of -20℃ to 60℃.

[0180] Dimensional variation: ≤0.1%

[0181] Resistance change: ≤2%

[0182] Mechanical properties: No significant change

[0183] 2. Study on the impact of humidity

[0184] Tested under relative humidity conditions of 30%–90%:

[0185] Moisture absorption rate: ≤0.2%

[0186] Dimensional variation: ≤0.05%

[0187] Electrical properties: Stable

[0188] 3. Chemical resistance study

[0189] 3.1 Acid and base tolerance: No change within the pH range of 3-10.

[0190] Under extreme pH conditions: slight effect

[0191] 3.2 Solvent resistance

[0192] Ethanol: No effect; Isopropanol: No effect; Acetone: Slight swelling

[0193] Example 7: Production Process Validation

[0194] This embodiment verifies the processing performance of the material under large-scale production conditions.

[0195] 1. Continuous production testing

[0196] 1.1 Production Equipment

[0197] Automatic screen printing machine: 8 stations

[0198] Curing oven: 10-meter tunnel type; Environmental control: Class 10,000 cleanroom throughout.

[0199] 1.2 Production Process Parameters: Printing Speed: 1200 pieces / hour

[0200] Curing conditions: 90℃, 20 minutes

[0201] Yield: ≥98.5%

[0202] 2. Batch consistency verification

[0203] 2.1 Testing of three production batches

[0204] Batch #CM001: Yield rate 98.7%

[0205] Batch #CM002: Yield rate 98.9%

[0206] Batch #CM003: Yield rate 98.6%

[0207] 2.2 Performance consistency viscosity deviation: ≤5%

[0208] Color consistency: ΔE≤1.5

[0209] Performance consistency: ≥98%

[0210] 3. Cost Analysis

[0211] 3.1 Material Costs: Raw material costs reduced by 15%.

[0212] Production costs: reduced by 20%

[0213] Overall cost: reduced by 18%

[0214] Example 8: Clinical Application Validation

[0215] This embodiment verifies the reliability of the material through actual clinical application.

[0216] 1. Hospital trial

[0217] 1.1 Trial Unit

[0218] Trial period at three tertiary-level hospitals: 6 months; Sample size: 5000 cases

[0219] 1.2 Trial Results

[0220] Operational error rate: reduced by 60%

[0221] Detection accuracy: Improved by 5%

[0222] User satisfaction: 95%

[0223] 2. Long-term tracking

[0224] 2.1 Performance Tracking

[0225] 6-month performance retention rate: ≥98%

[0226] Failure rate: ≤0.1%

[0227] Maintenance costs: reduced by 30%

[0228] Through system verification of the above embodiments, the isolation layer material formulation of the present invention has the following significant technical effects:

[0229] Excellent resistance to biological corrosion: After immersion in hemolyzed blood at 37°C for 24 hours, there is no swelling or exudation, and the weight change is ≤0.1%, which is significantly better than traditional materials.

[0230] Excellent electrical stability: resistance change ≤1% upon contact with system solution, volume resistivity ≥10. 15 Ω·cm provides a stable working environment for the sensor.

[0231] Good process applicability: viscosity is controlled at 4500±500 cPs, suitable for high-speed screen printing process, with a production efficiency of 1200 pieces / hour.

[0232] Excellent batch consistency: The yield rate of all three production batches is ≥98.5%, and the performance consistency is ≥98%, meeting the requirements of industrial production.

[0233] Wide environmental adaptability: Maintains stable performance in a temperature range of -20℃ to 60℃ and a humidity range of 30% to 90%.

[0234] Excellent compatibility: It exhibits good compatibility with all functional layers of the sensor (conductive path, electrode, enzyme layer) and does not affect the sensor performance.

[0235] Significant cost advantages: The overall cost is reduced by 18% compared to traditional materials, resulting in significant economic benefits.

[0236] Reliable clinical performance: It performs excellently in actual clinical applications, with a 60% reduction in operational error rate and a user satisfaction rate of 95%.

[0237] Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. Isolation layer material formulation characterized in that, The isolation layer material is composed of 118-08 type epoxy resin and phthalocyanine blue BGS colorant, and the material has no swelling or exudation after contacting 37℃ hemolytic blood sample for 24 hours, and the resistance change is ≤1% when contacting with system solution.

2. The spacer layer material formulation of claim 1, wherein: The isolation layer material is a 2k-epoxy resin system, which has solvent stability, chemical corrosion resistance, and is compatible with screen-printed electrode material and conductive path material.

3. The spacer layer material formulation of claim 1, wherein: The isolation layer material is a blue identification material, and the color component is phthalocyanine blue BGS, and the content is 0.5%-1.5% of the total amount of resin.

4. The spacer layer material formulation of claim 1, wherein: The isolation layer material further comprises a leveling agent, which is an organic silicon leveling agent BYK-333, and the addition amount is 0.1%-0.5% of the total amount of resin.

5. The spacer layer material formulation of claim 1, wherein: The isolation layer material further comprises a defoaming agent, which is an organic silicon defoaming agent BYK-055, and the addition amount is 0.05%-0.2% of the total amount of resin.

6. The spacer layer material formulation of claim 1, wherein: The viscosity of the isolation layer material is 3000-5000 cPs (25℃), which is suitable for screen printing process.

7. The spacer layer material formulation of claim 1, wherein: The curing condition of the isolation layer material after screen printing is: temperature 80-100℃, time 10-30 minutes. The thickness of the isolation layer formed after curing of the isolation layer material is 20-50μm.

8. The spacer layer material formulation of claim 1, wherein: The isolation layer material further comprises a dispersing agent, which is a high molecular dispersing agent BYK-163, and the addition amount is 0.1%-0.3% of the total amount of resin.

9. A biosensor isolation layer, characterized by, Prepared from the isolation layer material formulation of any one of claims 1-8.

10. A biosensor characterized by, Comprising the biosensor isolation layer of claim 9. Comprising the biosensor isolation layer of claim 9.