CN116604221A - A kind of infrared detection window solder material and preparation method thereof - Google Patents

Abstract

An infrared detection window solder material and a preparation method thereof relate to the field of solder materials and solve the problem that the existing solder is harmful to the environment and health. The solder material comprises the following components in parts by mass: tin: 80-97 parts of silver: 2.5-10 parts of copper: 0.3-5 parts of nano material: 2-5 parts of ethylene glycol: 1-2 parts. The preparation method comprises the following steps: weighing and mixing tin, silver and copper in proportion; weighing nano materials, and uniformly mixing the nano materials with the materials; adding the mixed materials into a vacuum smelting furnace, firstly filling nitrogen, then vacuumizing, heating to a specific temperature, and magnetically stirring; carrying out water quenching treatment on the mixture, cooling and drying under the protection of nitrogen; and weighing the ethylene glycol according to a proportion, heating to melt, adding the prepared silver-copper solder into the ethylene glycol, uniformly mixing, cooling and vacuum packaging. The invention can be applied to welding of various metals and alloy materials such as gold, silver, copper, nickel, zinc and the like, and has wide application prospect.

Description

A kind of infrared detection window solder material and preparation method thereof

technical field

The invention relates to the technical field of solder, in particular to an infrared detection window solder material and a preparation method thereof.

Background technique

Infrared detection window welding, the metallized window parts and shell parts are welded by fusion sealing with welding materials. In order to obtain a highly airtight and highly reliable infrared detection window, high-performance soldering materials are one of the keys.

At present, tin solder is widely used, which is generally composed of tin, lead, antimony and flux, and has a good soldering effect. However, lead and antimony are toxic and harmful substances, which affect the health of operators; in addition, conventional tin solder needs to be used with flux to achieve a good welding effect. The use of flux increases the complexity of the welding process, and the addition of tooling is time-consuming and laborious. Cleaning is complicated, time-consuming, costly, and harmful to the environment and human health.

Therefore, there is an urgent need to develop a tin solder that does not contain lead and antimony and can achieve good soldering effects without using flux, which is of great significance for environmentally friendly production and applications, as well as for the health of operators.

Contents of the invention

In order to solve the problem that the existing solder material is harmful to the environment and health, the invention proposes an infrared detection window solder material and a preparation method thereof.

Technical scheme of the present invention is as follows:

An infrared detection window solder material, comprising the following components in parts by mass:

Tin: 80-97 parts, silver: 2.5-10 parts, copper: 0.3-5 parts, nanomaterials: 2-5 parts, ethylene glycol: 1-2 parts.

Preferably, the nanomaterial is one or a mixture of at least two of nanoscale carbon powder, aluminum powder, and titanium dioxide.

Preferably, the particle diameters of the silver and copper are both D50=5nm~10μm.

Preferably, the particle size of the nanomaterial is D50=5nm~100nm.

A preparation method of the above-mentioned infrared detection window solder material, comprising the steps of:

S1, tin, silver and copper are weighed and mixed in proportion;

S2. Weighing the nanometer material and mixing it evenly with the material in step S1;

S3. Put the mixed materials into the vacuum melting furnace, first fill with nitrogen, then vacuumize, heat to a specific temperature, and magnetically stir;

S4. Carry out water quenching treatment to the mixture obtained in step S3, and dry under the protection of nitrogen after cooling;

S5. Weigh the ethylene glycol in proportion, heat to melt, add the prepared silver-copper solder into the ethylene glycol, mix evenly, and vacuum pack after cooling.

Preferably, the vacuum degree after vacuuming in step S3 is not higher than 5×10 ^-2 Pa, the specific temperature is 300°C-350°C, and the vacuum degree after heating is maintained at 2Pa-125Pa.

Preferably, the magnetic stirring time in step S3 is 10 min to 30 min.

Preferably, the temperature after cooling in step S4 is 25°C-45°C.

Preferably, the heating temperature in step S5 is 50°C-60°C.

Compared with prior art, concrete beneficial effect of the present invention is:

1. The present invention provides a new type of flux-free tin solder containing silver-copper components and nano-materials, which is lead-free and antimony-free. During the soldering process, the tin solder is heated to a molten state, and the nano-material reducing agent will Tin oxide and copper oxide are reduced to simple tin and copper, real-time reduction, removal of oxides, exemption from the use of flux, convenient application, reduction of smoke and harmful volatiles, good welding performance and wide application prospects, and good for environmental protection and human body health is important;

2. The addition of ethylene glycol in the infrared detection window solder material provided by the present invention can not only act as a solvent, reduce the surface tension of the tin solder when it melts, make the tin solder easier to spread, strengthen and improve the welding quality and efficiency, but also can Form a layer of diaphragm, to a certain extent, prevent the contact between air and tin solder, and delay the secondary oxidation; ethylene glycol can also react with oxygen to generate a small amount of formic acid and acetic acid, which can remove oxides and improve wettability; There is no residue after the diol is volatilized by heat, and no cleaning is required;

3. In the infrared detection window solder material provided by the present invention, the melting point of nanoscale silver and copper powder itself is lower than that of macroscale, while molten tin can form alloys with micro-nanoscale silver and copper, so the process of tin-silver-copper mixed smelting can be extremely Greatly reduce the production temperature, which is beneficial to energy saving and increase production efficiency and cost;

4. Nanomaterials are selected from nanoscale carbon powder, aluminum powder, titanium dioxide, or a mixture of at least two of them. Carbon and aluminum can react with oxidized components in the solder and reduce them to metal tin, silver and copper, preventing tin solder Oxidation, and nano-scale carbon and aluminum materials, due to small particle size, large specific surface area, large number of surface atoms, insufficient atomic coordination and high surface energy, the surface atoms have high activity and are very easy to combine with other atoms , so the above reaction is very easy to carry out; the nanoparticles are small, easy to disperse, and can be more fully in contact with the solder material of the infrared detection window, and are not easy to affect the overall performance of the solder; nano-titanium dioxide has a catalytic sensitization effect and improves the reduction reaction activity;

5. The preparation method of the present invention is simple, easy for industrial production, and can be applied to the welding of various metals and alloy materials such as gold, silver, copper, nickel, zinc, etc., and has wide application prospects.

Description of drawings

FIG. 1 is a schematic diagram of sample welding using welding materials in Example 1.

Detailed ways

In order to make the technical solution of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the accompanying drawings of the present invention. It should be noted that the following examples are only for better understanding The technical solution of the present invention should not be construed as a limitation of the present invention.

Example 1.

Weigh 90g of tin, 3.5g of silver and 2g of copper metal material and mix together, wherein silver and copper adopt high-purity nanometer powder with a particle size of 20nm;

Weigh 2g of carbon powder, 1g of aluminum powder and 0.5g of titanium dioxide and mix evenly, with a particle size of 10nm;

Put the mixed material into the vacuum melting furnace, fill it with nitrogen, and then evacuate, the vacuum degree reaches 5×10 ^-2 Pa, heat and control the temperature to 300°C, keep the vacuum degree at 5 Pa, and vacuum magnetically stir for 20 minutes;

The obtained mixture was subjected to water quenching treatment, then cooled to 30° C., and dried under nitrogen protection;

Weigh 1g of ethylene glycol, heat to 55°C to melt the ethylene glycol, add the prepared silver-copper solder into the ethylene glycol, mix well, and vacuum pack after cooling.

Example 2.

Weigh 80g of tin, 2.5g of silver and 1g of copper metal material and mix together, wherein silver and copper adopt high-purity nanometer powder with a particle size of 10nm;

Weigh 1g of carbon powder, 0.5g of aluminum powder and 0.5g of titanium dioxide and mix evenly, with a particle size of 8nm;

Put the mixed material into the vacuum melting furnace, fill it with nitrogen, and then evacuate, the vacuum degree reaches 5×10 ^-2 Pa, heat and control the temperature to 300°C, keep the vacuum degree at 5 Pa, and vacuum magnetically stir for 20 minutes;

The obtained mixture was subjected to water quenching treatment, then cooled to 30° C., and dried under nitrogen protection;

Weigh 1g of ethylene glycol, heat to 55°C to melt the ethylene glycol, add the prepared silver-copper solder into the ethylene glycol, mix well, and vacuum pack after cooling.

Example 3.

Take by weighing 95g tin, 5g silver and 4g copper metal material and mix together, wherein silver and copper adopt the high-purity nano-powder of particle size 20nm;

Weigh 3g of carbon powder, 1.5g of aluminum powder and 0.5g of titanium dioxide and mix evenly, with a particle size of 10nm;

Put the mixed material into the vacuum melting furnace, fill it with nitrogen, and then evacuate, the vacuum degree reaches 5×10 ^-2 Pa, heat and control the temperature to 300°C, keep the vacuum degree at 5 Pa, and vacuum magnetically stir for 20 minutes;

The obtained mixture was subjected to water quenching treatment, then cooled to 30° C., and dried under nitrogen protection;

Weigh 2g of ethylene glycol, heat to 55°C to melt the ethylene glycol, add the prepared silver-copper solder into the ethylene glycol, mix well, and vacuum pack after cooling.

Effect example.

The infrared detection window welding material prepared in Example 1 was used for sample welding. The welding area is shown in Figure 1. It can be seen from the figure that the welding area is fully filled and completely wetted and covered.

After sample welding of the welding materials prepared in Examples 1-3, the gas-tightness helium mass spectrometry test was carried out at 25°C and the pressure difference on both sides was 100kPa. The test results are shown in Table 1, and the leakage rate is low. At 10 ^-14 Pa.m ³ /s, it can be proved that the performance of the solder is reliable.

Table 1

Example 1 Example 2 Example 3 Leak rate/Pa.m3/s 3.26×10-15Pa.m3/s 7.90×10-15Pa.m3/s 6.54×10-15Pa.m3/s

The melting point of nano-scale silver and copper powder in the infrared detection window solder material is lower than that of the macro scale, while molten tin can form an alloy with micro-nano scale silver and copper, so the production temperature can be greatly reduced during the mixed melting process of tin, silver and copper, which is beneficial Energy saving and increase production efficiency and cost;

The nano-materials in the infrared detection window solder material are selected from one or at least two mixed materials of nano-scale carbon powder, aluminum powder, and titanium dioxide. Carbon and aluminum can react with the oxidized components in the solder and reduce them to metal tin, silver, and copper. , to prevent the oxidation of tin solder, SnO ₂ +C=Sn+CO ₂ ↑, 3CuO+2Al=3Cu+Al ₂ O ₃ , the density of alumina is 3.9g/cm ³ ~4.0g/cm ³ , and the density of common solder is >7g /cm ³ , so the generated Al ₂ O ₃ will float on the surface without affecting welding;

Moreover, due to the small particle size, large specific surface area, large number of surface atoms, insufficient atomic coordination and high surface energy of nano-scale carbon and aluminum materials, the surface atoms have high activity and are easily combined with other atoms. The above reaction is very easy to carry out; the nanoparticles are small, easy to disperse, can more fully contact with the solder material of the infrared detection window, and are not easy to affect the overall performance of the solder; nano-titanium dioxide has a catalytic sensitization effect and improves the reduction reaction activity.

Claims (9)

1. An infrared detection window solder material, characterized in that, comprises the following components in parts by mass: Tin: 80-97 parts, silver: 2.5-10 parts, copper: 0.3-5 parts, nanomaterials: 2-5 parts, ethylene glycol: 1-2 parts. 2 . The infrared detection window solder material according to claim 1 , wherein the nanomaterial is one or a mixture of at least two of nanoscale carbon powder, aluminum powder, and titanium dioxide. 3 . The infrared detection window solder material according to claim 1 , wherein the particle diameters of the silver and copper are both D50=5nm˜10 μm. 4. The infrared detection window solder material according to claim 1, characterized in that, the particle size of the nanomaterial is D50=5nm~100nm. 5. A method for preparing the infrared detection window solder material according to any one of claims 1-4, characterized in that, comprising the steps of: S1, tin, silver and copper are weighed and mixed in proportion; S2. Weighing the nanometer material and mixing it evenly with the material in step S1; S3. Put the mixed materials into the vacuum melting furnace, first fill with nitrogen, then vacuumize, heat to a specific temperature, and magnetically stir; S4. Carry out water quenching treatment to the mixture obtained in step S3, and dry under the protection of nitrogen after cooling; S5. Weigh the ethylene glycol in proportion, heat to melt, add the prepared silver-copper solder into the ethylene glycol, mix evenly, and vacuum pack after cooling. 6. The preparation method of the infrared detection window solder material according to claim 5, characterized in that, in step S3, the degree of vacuum after vacuuming is not higher than 5×10 ^-2 Pa, and the specific temperature is 300°C ~350°C, the vacuum degree after the heating is kept at 2Pa~125Pa. 7 . The method for preparing the solder material for the infrared detection window according to claim 5 , wherein the magnetic stirring time in step S3 is 10 minutes to 30 minutes. 8 . The method for preparing an infrared detection window solder material according to claim 5 , wherein the temperature after cooling in step S4 is 25° C. to 45° C. 8 . 9 . The method for preparing the solder material for the infrared detection window according to claim 5 , wherein the heating temperature in step S5 is 50° C. to 60° C. 9 .