Quantitative analysis method for harmful superfine powder in electrolytic copper powder for electrical alloy

Abstract

The invention belongs to the technical field of metal powder and detection, and particularly relates to a quantitative analysis method for harmful superfine powder in electrolytic copper powder for electrical alloy. The technology comprises the following steps: S1, placing electrolytic copper powder to be detected in deionized water, carrying out dispersion treatment through ultrasonic and magnetic stirring, controlling the frequency, power and dispersion time of ultrasonic, and controlling the rotating speed and dispersion time of magnetic stirring, so that the electrolytic copper powder is uniformly dispersed in water; s2, separating and drying to obtain uniformly dispersed electrolytic copper powder particles; and S3, harmful superfine powder and electrolytic copper powder with normal particle size are screened out, and the proportion of the harmful superfine powder is calculated. Electrolytic copper powder is dispersed in a dispersion medium through an ultrasonic and magnetic stirring technology, accurate calculation of the content of harmful superfine powder is achieved through a drying and weighing method, and the method is easy and convenient to operate and accurate in result.

Description

Technical Field

[0001] The invention belongs to the technical field of metal powder and detection, and in particular relates to a quantitative analysis method of harmful ultrafine powder in electrolytic copper powder for electrical alloy. Background Art

[0002] The performance of electrical alloys depends largely on the quality of its raw material - electrolytic copper powder. The presence of harmful ultrafine powder (usually refers to powder particles with a particle size less than a certain threshold) not only affects the uniformity and stability of the alloy, but may also lead to a decrease in electrical performance and weakened mechanical strength. Therefore, accurate detection of harmful ultrafine powder in electrolytic copper powder is a key step to ensure the quality of electrical alloys.

[0003] Existing analytical methods usually use chemical or physical methods, but they have disadvantages such as cumbersome operations, long time consumption, and inaccurate results. Summary of the invention

[0004] The purpose of the present invention is to provide a method for quantitatively analyzing harmful ultrafine powder in electrolytic copper powder for electrical alloy, which can at least realize effective separation and measurement of harmful ultrafine powder.

[0005] The method for quantitatively analyzing harmful ultrafine powder in electrolytic copper powder for electrical alloy comprises the following steps:

[0006] S1: placing the electrolytic copper powder to be tested in deionized water, dispersing it by ultrasonic and magnetic stirring, controlling the frequency, power and dispersion time of the ultrasonic wave, and controlling the speed and dispersion time of the magnetic stirring, so that the electrolytic copper powder is evenly dispersed in the water;

[0007] S2: separation and drying to obtain uniformly dispersed electrolytic copper powder particles;

[0008] S3: Screen out harmful ultrafine powder and electrolytic copper powder of normal particle size, and calculate the proportion of harmful ultrafine powder.

[0009] Furthermore, in step S1, the electrolytic copper powder to be detected is 5g to 15g, and the deionized water is 150ml to 450ml.

[0010] Furthermore, in the step S1, an ultrasonic dispersing device and a magnetic stirring dispersing device are used for dispersing treatment.

[0011] Furthermore, in step S1, the ultrasonic dispersion device has an ultrasonic frequency of 20kHz to 40kHz and a power of 100W to 300W.

[0012] Furthermore, in step S1, the rotation speed of the magnetic stirring dispersion device is 1000 rpm / min to 2000 rpm / min.

[0013] Furthermore, in step S1, when the ultrasonic wave and magnetic stirring are used for dispersion treatment, ultrasonic dispersion is performed first and then magnetic stirring dispersion is performed, or magnetic stirring dispersion is performed first and then ultrasonic dispersion is performed;

[0014] When ultrasonic dispersion is first performed and then magnetic stirring dispersion is performed, the ultrasonic dispersion time is 10min to 20min, and the magnetic stirring dispersion time is 5min to 15min;

[0015] When magnetic stirring dispersion is performed first and then ultrasonic dispersion is performed, the magnetic stirring dispersion time is 10 minutes to 20 minutes, and the ultrasonic dispersion time is 5 minutes to 15 minutes.

[0016] Furthermore, in step S2, vacuum drying is used for drying, the vacuum drying temperature is 40° C. to 80° C., and the drying time is 10 min to 35 min.

[0017] Furthermore, in step S3, the aperture of the sieve during screening is 40 μm to 50 μm.

[0018] Furthermore, the method further comprises step S4: performing chemical composition analysis on the sieved harmful ultrafine powder.

[0019] Compared with the prior art, the present invention has the following beneficial effects:

[0020] The electrolytic copper powder is dispersed in the dispersion medium by ultrasonic and magnetic stirring technology, and the content of harmful ultrafine powder is accurately calculated by drying and weighing methods. This method is simple to operate and has accurate results, providing an effective technical means for controlling the quality of electrolytic copper powder in the electrical alloy industry. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] Figure 1 A schematic diagram of an ultrasonic dispersion device used in a method for quantitatively analyzing harmful ultrafine powder in electrolytic copper powder for electrical alloys;

[0022] Figure 2 The present invention is a schematic diagram of a magnetic stirring and dispersing device used in a quantitative analysis method of harmful ultrafine powder in electrolytic copper powder for electrical alloys.

[0023] Names of components in the figure: 1. Ultrasonic dispersion device; 2. Magnetic stirring dispersion device. DETAILED DESCRIPTION

[0024] The present invention is further described below through specific embodiments in conjunction with the accompanying drawings, but the present invention is not limited thereto. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

[0025] The method for quantitatively analyzing harmful ultrafine powder in electrolytic copper powder for electrical alloy described in this embodiment comprises the following steps:

[0026] S1: Place the electrolytic copper powder to be tested in deionized water, and disperse it by ultrasonic and magnetic stirring. Control the frequency, power, and dispersion time of the ultrasonic wave, and control the speed and dispersion time of the magnetic stirring to make the electrolytic copper powder evenly dispersed in the water.

[0027] Among them, the electrolytic copper powder to be tested is 5g to 15g, the deionized water is 150ml to 450ml, and the ultrasonic dispersion device 1 and the magnetic stirring dispersion device 2 are used for dispersion treatment. The ultrasonic dispersion device 1 adopts the Jiemeng brand ultrasonic cleaning machine of Shenzhen Jiemeng Cleaning Equipment Co., Ltd., model JP-060; the magnetic stirring dispersion device 2 adopts the Yuhua 85-1B magnetic stirrer of Gongyi Yuhua Instrument Co., Ltd. Ultrasonic dispersion can be performed first, and then magnetic stirring. When ultrasonic dispersion is performed first and then magnetic stirring is performed, the ultrasonic frequency of the ultrasonic dispersion device 1 is 20kHz to 40kHz, the power is 100W to 300W, and the dispersion time is 10min to 20min, and then magnetic stirring is performed. The rotation speed of the magnetic stirring dispersion device 2 is 1000rpm / min to 2000rpm / min, and the dispersion time is 5min to 15min. Alternatively, magnetic stirring may be performed first, followed by ultrasonic dispersion. When magnetic stirring is performed first and then ultrasonic dispersion is performed, the ultrasonic frequency of the ultrasonic dispersion device 1 is 20kHz to 40kHz, the power is 100W to 300W, the dispersion time is 5min to 15min, the rotation speed of the magnetic stirring dispersion device 2 is 1000rpm / min to 2000rpm / min, and the dispersion time is 10min to 20min. Ultrasonic dispersion devices 1 and magnetic stirring dispersion devices 2 of other manufacturers and other models with the same functions may also be used.

[0028] The electrolytic copper powder for the electrical alloy to be tested is evenly placed in a certain amount of deionized water, and the ultrasonic dispersion device 1 is used to perform high-frequency vibration treatment on the electrolytic copper powder to be tested, so that the electrolytic copper powder particles are evenly dispersed in the water to form a stable ultrafine powder. The high-frequency vibration is optimized according to the specific characteristics of the electrolytic copper powder, and the dispersion time, frequency and power of the ultrasonic dispersion device 1 are controlled to achieve the best dispersion effect. At the same time, the magnetic stirring dispersion device 2 is used to magnetically stir the electrolytic copper powder to be tested, which further promotes the dispersion of the electrolytic copper powder.

[0029] S2: separation and drying to obtain uniformly dispersed electrolytic copper powder particles;

[0030] Dry the evenly dispersed suspended electrolytic copper powder in step S1: filter the mixture after ultrasonic and magnetic stirring treatment, separate the electrolytic copper powder suspended in the dispersion medium, transfer the electrolytic copper powder to a drying device, and use vacuum drying technology to dry it to remove moisture and retain evenly dispersed electrolytic copper powder particles. When using a vacuum drying oven for drying, the vacuum drying temperature is 40°C to 80°C, and the drying time is 10min to 35min. The drying process requires strict control of temperature and humidity, and the relative humidity is controlled to be ≦85% rh to avoid re-agglomeration of copper powder particles. During the drying process, an ordinary drying oven can also be used, and the drying temperature is controlled at 115°C to 125°C, and the drying time is 20min to 60min.

[0031] S3: Screen out harmful ultrafine powder and electrolytic copper powder of normal particle size, and calculate the proportion of harmful ultrafine powder.

[0032] The sieve mesh size during screening is 40μm to 50μm. The harmful ultrafine powder and electrolytic copper powder with normal particle size are screened out and then weighed and analyzed.

[0033] The harmful ultrafine powder is separated from the electrolytic copper powder of normal particle size by using a sieve with a specific aperture, and the weight of the harmful ultrafine powder and the electrolytic copper powder of normal particle size are weighed respectively. Then, by calculating the proportion of the mass of the harmful ultrafine powder to the total mass, the content of the harmful ultrafine powder in the electrolytic copper powder can be obtained.

[0034] S4: Analyze the harmful ultrafine powders screened out to evaluate their impact on the properties of electrical alloys.

[0035] According to actual needs, the chemical composition of harmful ultrafine powders can be further analyzed to evaluate their specific impact on the performance of electrical alloys, and the production process or screening standards of electrolytic copper powder can be adjusted accordingly to achieve quality control of electrolytic copper powder for electrical alloys.

[0036] Ultrasonic and magnetic stirring techniques are used to disperse electrolytic copper powder in the dispersion medium to achieve effective separation and measurement of harmful ultrafine powders. By combining ultrasonic dispersion with precise weighing technology, the content of harmful ultrafine powders can be quickly and accurately determined.

[0037] This embodiment proposes a new quantitative analysis method, which uses high-frequency vibration technology to disperse electrolytic copper powder in a dispersion medium to achieve effective separation and measurement of harmful ultrafine powders, and combines ultrasonic dispersion with precise weighing technology to achieve rapid and accurate determination of the content of harmful ultrafine powders.

[0038] A quantitative analysis method for harmful ultrafine powder in electrolytic copper powder for electrical alloy has the following advantages: 1. Easy operation: The electrolytic copper powder can be quickly and evenly dispersed in the dispersion medium by using ultrasonic and magnetic stirring technology, which simplifies the operation steps. 2. Accurate results: The content of harmful ultrafine powder can be accurately calculated by drying and weighing methods, which improves the accuracy of analysis. 3. Wide range of applications: This method is applicable to electrolytic copper powders of different particle sizes and compositions, and has high versatility.

[0039] Example 1

[0040] S1: Take 10g of electrolytic copper powder for electrical alloy and add it into a beaker of 300mL deionized water; use an ultrasonic dispersion device 1 with a frequency of 40kHz and a power of 100W to treat for 10min, and use a magnetic stirring dispersion device 2 with a speed of 1500rpm / min to magnetically stir the electrolytic copper powder for 10min.

[0041] S2: Filter the mixture after the ultrasonic and magnetic stirring treatment to separate the electrolytic copper powder suspended in the dispersion medium, transfer the electrolytic copper powder to a drying device, and dry it in a vacuum drying oven at 60° C. for 30 minutes.

[0042] S3: After drying, the dried electrolytic copper powder is screened using a 45 μm pore size sieve to separate harmful ultrafine powder.

[0043] S4: Weigh the harmful ultrafine powder and the electrolytic copper powder with normal particle size respectively, and calculate the content percentage of the harmful ultrafine powder.

[0044] The following table is Table 1, which records the weight and content of harmful ultrafine powder in the electrolytic copper powder obtained by weighing 10g of electrolytic copper powder for electrical alloy and using a quantitative analysis method for harmful ultrafine powder in electrolytic copper powder for electrical alloy according to this embodiment.

[0045] Table 1:

[0046] Serial number Initial weight / g Weight of harmful ultrafine powder / g Harmful ultrafine powder content / % 1 10.0 0.0120 0.12 2 10.0 0.0075 0.075 3 10.0 0.0082 0.082 4 10.0 0.0111 0.111 5 10.0 0.0098 0.098 6 10.0 0.0077 0.077 7 10.0 0.0101 0.101 8 10.0 0.0083 0.083 9 10.0 0.0092 0.092 10 10.0 0.0073 0.073 11 10.0 0.0104 0.104 12 10.0 0.0088 0.088 13 10.0 0.0089 0.089

[0047] Example 2

[0048] S1: Take 15g of electrolytic copper powder for electrical alloy and add it to a beaker of 450mL deionized water; use an ultrasonic dispersion device 1 with a frequency of 40kHz and a power of 200W to treat it for 15min, and use a magnetic stirring dispersion device 2 with a speed of 2000rpm / min to magnetically stir the electrolytic copper powder for 10min.

[0049] S2: filtering the mixture after the ultrasonic and magnetic stirring treatment to separate the electrolytic copper powder suspended in the dispersion medium, transferring the electrolytic copper powder to a drying device, and drying it in a vacuum drying oven at 80° C. for 20 minutes.

[0050] S3: After drying, the dried electrolytic copper powder is screened using a 40 μm pore size sieve to separate harmful ultrafine powder.

[0051] S4: Weigh the harmful ultrafine powder and the electrolytic copper powder with normal particle size respectively, and calculate the content percentage of the harmful ultrafine powder.

[0052] The following table is Table 2, which records the weight and content of harmful ultrafine powder in the electrolytic copper powder obtained by weighing 15g of electrolytic copper powder for electrical alloy and using a quantitative analysis method for harmful ultrafine powder in electrolytic copper powder for electrical alloy according to this embodiment.

[0053] Table 2:

[0054] Serial number Initial weight / g Weight of harmful ultrafine powder / g Harmful ultrafine powder content / % 1 15 0.0176 0.117 2 15 0.0124 0.083 3 15 0.0165 0.110 4 15 0.0141 0.094 5 15 0.0166 0.111 6 15 0.0150 0.100 7 15 0.0153 0.102 8 15 0.0161 0.107 9 15 0.0144 0.096 10 15 0.0132 0.088 11 15 0.0136 0.091 12 15 0.0117 0.078 13 15 0.0133 0.089

[0055] Example 3

[0056] S1: Take 5g of electrolytic copper powder for electrical alloy and add it into a 150mL beaker of deionized water; use an ultrasonic dispersion device 1 with a frequency of 20kHz and a power of 100W to treat it for 15min, and use a magnetic stirring dispersion device 2 with a speed of 1000rpm / min to magnetically stir the electrolytic copper powder for 5min.

[0057] S2: filtering the mixture after the ultrasonic and magnetic stirring treatment to separate the electrolytic copper powder suspended in the dispersion medium, transferring the electrolytic copper powder to a drying device, and drying it in a vacuum drying oven at 45° C. for 10 minutes.

[0058] S3: After drying, the dried electrolytic copper powder is screened using a sieve with an aperture of 50 μm to separate harmful ultrafine powder.

[0059] S4: Weigh the harmful ultrafine powder and the electrolytic copper powder with normal particle size respectively, and calculate the content percentage of the harmful ultrafine powder.

[0060] Table 3:

[0061] Serial number Initial weight / g Weight of harmful ultrafine powder / g Harmful ultrafine powder content / % 1 5 0.0065 0.130 2 5 0.0054 0.108 3 5 0.0041 0.082 4 5 0.0035 0.070 5 5 0.0038 0.076 6 5 0.0039 0.078 7 5 0.0051 0.102 8 5 0.0048 0.096 9 5 0.0058 0.116 10 5 0.0054 0.108 11 5 0.0060 0.120 12 5 0.0039 0.078 13 5 0.0047 0.094

[0062] Table 3 records the weight and content of harmful ultrafine powder in electrolytic copper powder for electrical alloy obtained by weighing 5 g of electrolytic copper powder for electrical alloy and using a quantitative analysis method for harmful ultrafine powder in electrolytic copper powder for electrical alloy according to this embodiment.

Claims

1. A method for quantitative analysis of harmful ultrafine powder in electrolytic copper powder for electrical alloy, characterized in that: The following steps are involved: S1: placing the electrolytic copper powder to be tested in deionized water, dispersing it by ultrasonic and magnetic stirring, controlling the frequency, power and dispersion time of the ultrasonic wave, and controlling the speed and dispersion time of the magnetic stirring, so that the electrolytic copper powder is evenly dispersed in the water; S2: separation and drying to obtain uniformly dispersed electrolytic copper powder particles; S3: Screen out harmful ultrafine powder and electrolytic copper powder of normal particle size, and calculate the proportion of harmful ultrafine powder.

2. The method for quantitatively analyzing harmful ultrafine powder in electrolytic copper powder for electrical alloy according to claim 1, characterized in that: In the step S1, the electrolytic copper powder to be tested is 5g to 15g, and the deionized water is 150ml to 450ml.

3. The method for quantitatively analyzing harmful ultrafine powder in electrolytic copper powder for electrical alloy according to claim 1 or 2, characterized in that: In the step S1, an ultrasonic dispersion device (1) and a magnetic stirring dispersion device (2) are used to perform dispersion treatment.

4. The method for quantitatively analyzing harmful ultrafine powder in electrolytic copper powder for electrical alloy according to claim 3, characterized in that: In the step S1, the ultrasonic frequency of the ultrasonic dispersion device (1) is 20 kHz to 40 kHz, and the power is 100 W to 300 W.

5. The method for quantitatively analyzing harmful ultrafine powder in electrolytic copper powder for electrical alloy according to claim 3 or 4, characterized in that: In the step S1, the rotation speed of the magnetic stirring dispersion device (2) is 1000 rpm / min to 2000 rpm / min.

6. The method for quantitatively analyzing harmful ultrafine powder in electrolytic copper powder for electrical alloy according to claim 4 or 5, characterized in that: In the step S1, when the ultrasonic and magnetic stirring are used for dispersion treatment, ultrasonic dispersion is performed first and then magnetic stirring dispersion is performed, or magnetic stirring dispersion is performed first and then ultrasonic dispersion is performed; When ultrasonic dispersion is first performed and then magnetic stirring dispersion is performed, the ultrasonic dispersion time is 10min to 20min, and the magnetic stirring dispersion time is 5min to 15min; When magnetic stirring dispersion is performed first and then ultrasonic dispersion is performed, the magnetic stirring dispersion time is 10 minutes to 20 minutes, and the ultrasonic dispersion time is 5 minutes to 15 minutes.

7. The method for quantitatively analyzing harmful ultrafine powder in electrolytic copper powder for electrical alloy according to any one of claims 1 to 6, characterized in that: In the step S2, vacuum drying is used for drying, the vacuum drying temperature is 40° C. to 80° C., and the drying time is 10 min to 35 min.

8. The method for quantitatively analyzing harmful ultrafine powder in electrolytic copper powder for electrical alloy according to claim 7, characterized in that: In the step S3, the aperture of the sieve during screening is 40 μm to 50 μm.

9. The method for quantitatively analyzing harmful ultrafine powder in electrolytic copper powder for electrical alloy according to any one of claims 1 to 8, characterized in that: The method further comprises step S4: performing chemical composition analysis on the sieved harmful ultrafine powder.

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