CN108927518A - Quickly prepare the direct powder rolling method of Cu-Ni-Si latten - Google Patents

Abstract

The direct powder rolling method for quickly preparing Cu-Ni-Si alloy thin plate disclosed by the present invention comprises the steps of: weighing Cu, Ni, Si powder and mixing, and then rolling into Cu-Ni-Si green plate; The Cu‑Ni‑Si green sheet is sintered in a hydrogen atmosphere, then sintered in an argon atmosphere, and finally the temperature of the furnace body drops to room temperature to obtain a Cu‑Ni‑Si alloy sheet. The direct powder rolling method of the present invention quickly prepares Cu-Ni-Si alloy thin plate, uses Cu, Ni and Si single-substance mixed powder as raw material, and rolls into a green plate with a certain thickness and strength by controlling the gap between the rolls of the rolling mill, and then Putting it into an atmosphere furnace for sintering can prepare a Cu-Ni-Si alloy sheet with better performance. The preparation process of this method is simple, the cost is low, and the prepared Cu-Ni-Si alloy sheet has good tensile properties .

Description

Direct Powder Rolling Method for Rapid Preparation of Cu-Ni-Si Alloy Sheets

technical field

The invention belongs to the technical field of alloy material preparation, and in particular relates to a direct powder rolling method for rapidly preparing Cu-Ni-Si alloy thin plates.

Background technique

Due to the advantages of high strength, high electrical conductivity, and no magnetocaloric effect, Cu-Ni-Si alloys are considered to be the most promising candidates to replace Cu-Be alloys and become the main candidate materials for new lead frames. At present, the mainstream preparation method of Cu-Ni-Si alloy sheet is the melting casting method. First, the alloy ingot is prepared by the traditional melting casting method or the alloy rod is prepared by the horizontal continuous casting method, and then the multi-pass thermomechanical processing (extrusion or Rolling) and cold rolling and finishing processes to process the block into plates. When Cu-Ni-Si alloys are prepared by traditional melting and casting methods, it is easy to form a network of non-conductive intermetallic compound phases on the copper grain boundaries, thereby affecting the alloy. Strength and conductivity, and the processing technology from ingot to thin plate is cumbersome, the cooling rate is slow, and the obtained structure is relatively coarse, which makes it difficult for subsequent thermal processing, and the whole process is complicated and the process flow is long. In addition, Cu-Ni-Si alloy sheets are prepared by sputtering, but the equipment is relatively expensive. Therefore, there is an urgent need for a new method to prepare Cu-Ni-Si alloy sheets, which can improve production efficiency while reducing production costs.

Contents of the invention

The object of the present invention is to provide a direct powder rolling method for rapidly preparing Cu-Ni-Si alloy thin plates, which reduces production cost and improves production efficiency compared with traditional preparation methods.

The technical scheme adopted in the present invention is: the direct powder rolling method of fast preparation Cu-Ni-Si alloy thin plate comprises the following steps:

Step 1, Mixing

Weighing Cu, Ni, and Si powders are mixed to obtain Cu-Ni-Si mixed powder;

Step 2, Rolling

rolling the Cu-Ni-Si mixed powder to obtain a Cu-Ni-Si green plate;

Step 3, atmosphere sintering

Sintering the Cu-Ni-Si green sheet firstly in a hydrogen atmosphere, then sintering in an argon atmosphere, and finally waiting for the temperature of the furnace body to drop to room temperature to obtain the Cu-Ni-Si alloy sheet.

Further, in the step 1, the Cu powder is electrolytic Cu powder, and the Si powder is single crystal Si powder.

Further, in the step 1, the average particle size of the Cu powder weighed is 20um, and the average particle size of the Ni powder and Si powder is 1um.

Further, in the step 1, according to mass percentage, the Ni powder weighed accounts for 7%-8% of the Cu-Ni-Si mixed powder, and the Si powder accounts for 1.5%-2% of the Cu-Ni-Si mixed powder. , the rest is Cu powder, and the sum of the mass percentages of the above raw materials is 100%.

Further, in the step 2, the Cu-Ni-Si mixed powder is rolled for two to three passes by using a powder rolling machine.

Preferably, in the step 3, the sintering temperature is 680°C-720°C under hydrogen atmosphere, the sintering temperature is 900°C-980°C under argon atmosphere, and the sintering time is 1h-1.5h.

The beneficial effect of the present invention is: the direct powder rolling method of the present invention rapidly prepares Cu-Ni-Si alloy thin plate, uses Cu, Ni and Si single-substance mixed powder as raw material, by controlling the roll gap of rolling mill to roll to have certain thickness and strength of the green plate, and then put it into the atmosphere furnace for sintering, the Cu-Ni-Si alloy plate with better performance can be prepared. The preparation process of this method is simple, the cost is low, and the prepared Cu-Ni-Si The alloy sheet has good tensile properties.

Description of drawings

Fig. 1 is the flow chart of the direct powder rolling method of fast preparation Cu-Ni-Si alloy thin plate of the present invention;

Fig. 2 is the scanning electron microscope contrast image of two kinds of Cu powder raw materials that the present invention adopts respectively;

Fig. 3 is the macroscopic morphology image of the Cu-Ni-Si green plate material after adopting different passes of rolling in the present invention;

Fig. 4 is the microstructure image of the Cu-Ni-Si alloy plate prepared after 900 DEG C under the argon atmosphere of the present invention;

Fig. 5 is the microstructure image of the Cu-Ni-Si alloy plate prepared after 950 DEG C under the argon atmosphere of the present invention;

Fig. 6 is a comparison chart of the tensile strength test of the Cu-Ni-Si alloy plate prepared by the present invention and the pure copper plate.

Detailed ways

The flow chart of the direct powder rolling method for the rapid preparation of Cu-Ni-Si alloy sheet provided by the present invention is shown in Figure 1, comprising the following steps:

Step 1, Mixing

Weighing Cu, Ni, and Si powders and mixing them to obtain Cu-Ni-Si mixed powders;

Further, the Cu powder is electrolytic Cu powder, and the Si powder is single crystal Si powder.

Further, the average particle diameter of Cu powder is 20um, and the average particle diameter of Ni powder and Si powder is 1um.

Preferably, in terms of mass percentage, the Ni powder to be weighed accounts for 7%-8% of the Cu-Ni-Si mixed powder, the Si powder accounts for 1.5%-2% of the Cu-Ni-Si mixed powder, and the rest is Cu powder, The sum of the mass percentages of the above raw materials is 100%.

Step 2, Rolling

Rolling the Cu-Ni-Si mixed powder two to three times to obtain a Cu-Ni-Si green plate;

Step 3, atmosphere sintering

Introduce hydrogen into the atmosphere furnace first, so that on the one hand, the oxygen in the furnace body can be eliminated, and on the other hand, the oxidized Cu particles in the Cu-Ni-Si green sheet can be reduced, and the Cu-Ni-Si green sheet can be placed in the Sintering in a hydrogen atmosphere, then sintering in an argon atmosphere, and finally the temperature of the furnace body drops to room temperature to obtain a Cu-Ni-Si alloy plate.

Specifically, the sintering temperature is 680°C-720°C under a hydrogen atmosphere, and 900°C-980°C under an argon atmosphere.

After sintering at a high temperature of 900°C-980°C in an argon atmosphere, the surface of the alloy sheet is smooth, and the edge of the sheet will not crack or curl.

The present invention will be described in detail below in conjunction with the accompanying drawings and specific embodiments.

Example 1

The direct powder rolling method for the rapid preparation of Cu-Ni-Si alloy sheet provided in this embodiment comprises the following steps:

Step 1, Mixing

Weigh 91.5g of gas-atomized Cu powder (purity above 99.9%, average particle diameter 20um), 7g pure Ni powder (purity above 99.9%, average particle diameter 1um), 1.5g single crystal Si powder (purity above 99.9%, average particle diameter particle size 1um) and mixed to obtain Cu-Ni-Si mixed powder; in this embodiment, the gas-atomized Cu powder is added in the powder mixer, and then vacuum pump oil and ZrO balls (ball material ₎ with 0.8% Cu quality are added The ratio is 1:4) and mix for 1h, then add Ni powder and single crystal Si powder and mix for 2h. In this step, it is only necessary to mix the three raw materials evenly, and the mixing method and mixing tools are not limited.

Step 2, Rolling

Put the Cu-Ni-Si mixed powder into the powder rolling mill for secondary rolling, and control the gap between the rolls by adjusting the fine screw on the rolling mill to obtain the Cu-Ni-Si green sheet; this embodiment controls The gap between the rolls is such that the thickness of the Cu-Ni-Si green sheet is 0.3 mm.

Step 3, atmosphere sintering

First put hydrogen into the atmosphere furnace, raise the temperature of the Cu-Ni-Si green sheet to 680°C for sintering in a hydrogen atmosphere, then put argon into the furnace body, raise the temperature to 900°C for sintering for 1.5h under an argon atmosphere , and finally when the temperature of the furnace body drops to room temperature, the Cu-Ni-Si alloy plate is obtained.

Example 2

The direct powder rolling method for the rapid preparation of Cu-Ni-Si alloy sheet provided in this embodiment comprises the following steps:

Step 1, Mixing

Weigh 91.2g electrolytic Cu elemental powder (purity above 99.9%, average particle diameter 20um), 7.3g pure Ni powder (purity above 99.9%, average particle diameter 1um), 1.5g single crystal Si powder (purity above 99.9%, average particle diameter particle size 1um) and mixed to obtain Cu-Ni-Si mixed powder; in this embodiment, first pure electrolytic Cu elemental powder is added in the powder mixer, and then vacuum pump oil and ZrO balls (balls ₎ with 0.8% electrolytic Cu mass are added The material ratio is 1:4) and mix for 1h, then add Ni powder and single crystal Si powder and mix for 2h. In this step, it is only necessary to mix the three raw materials evenly, and the mixing method and mixing tools are not limited.

Step 2, Rolling

Put the Cu-Ni-Si mixed powder into the powder rolling mill for three-pass rolling, and control the gap between the rolls by adjusting the fine screw on the rolling mill to obtain the Cu-Ni-Si green sheet; this embodiment controls The gap between the rolls is such that the thickness of the Cu-Ni-Si green sheet is 0.3mm.

Step 3, atmosphere sintering

First put hydrogen into the atmosphere furnace, raise the temperature of the Cu-Ni-Si green sheet to 690°C for sintering in a hydrogen atmosphere, then put argon into the furnace body, raise the temperature to 920°C for sintering in an argon atmosphere for 1.3h , and finally when the temperature of the furnace body drops to room temperature, the Cu-Ni-Si alloy plate is obtained.

Example 3

The direct powder rolling method for the rapid preparation of Cu-Ni-Si alloy sheet provided in this embodiment comprises the following steps:

Step 1, Mixing

Weigh 91g electrolytic Cu elemental powder (purity above 99.9%, average particle size 20um), 7.5g pure Ni powder (purity above 99.9%, average particle size 1um), 1.5g single crystal Si powder (purity above 99.9%, average particle size diameter 1um) and mixed to obtain Cu-Ni-Si mixed powder; in this embodiment, first pure electrolytic Cu elemental powder is added in the powder mixer, and then vacuum pump oil and ZrO balls (ball material ₎ with 0.8% electrolytic Cu mass are added The ratio is 1:4) and mix for 1h, then add Ni powder and single crystal Si powder and mix for 2h. In this step, it is only necessary to mix the three raw materials evenly, and the mixing method and mixing tools are not limited.

Step 2, Rolling

Put the Cu-Ni-Si mixed powder into the powder rolling mill for three-pass rolling, and control the gap between the rolls by adjusting the fine screw on the rolling mill to obtain the Cu-Ni-Si green sheet; this embodiment controls The gap between the rolls is such that the thickness of the Cu-Ni-Si green sheet is 0.3mm.

Step 3, atmosphere sintering

First put hydrogen into the atmosphere furnace, raise the temperature of the Cu-Ni-Si green sheet to 720°C for sintering in a hydrogen atmosphere, then put argon into the furnace body, raise the temperature to 950°C for sintering in an argon atmosphere for 1.2h , and finally when the temperature of the furnace body drops to room temperature, the Cu-Ni-Si alloy plate is obtained.

Example 4

The direct powder rolling method for the rapid preparation of Cu-Ni-Si alloy sheet provided in this embodiment comprises the following steps:

Step 1, Mixing

Weigh 90.4g electrolytic Cu elemental powder (purity above 99.9%, average particle diameter 20um), 7.8g pure Ni powder (purity above 99.9%, average particle diameter 1um), 1.8g single crystal Si powder (purity above 99.9%, average particle diameter particle size 1um) and mixed to obtain Cu-Ni-Si mixed powder; in this embodiment, first pure electrolytic Cu elemental powder is added in the powder mixer, and then vacuum pump oil and ZrO balls (balls ₎ with 0.8% electrolytic Cu quality are added The material ratio is 1:4) and mix for 1h, then add Ni powder and single crystal Si powder and mix for 2h. In this step, it is only necessary to mix the three raw materials evenly, and the mixing method and mixing tools are not limited.

Step 2, Rolling

Put the Cu-Ni-Si mixed powder into the powder rolling mill for secondary rolling, and control the gap between the rolls by adjusting the fine screw on the rolling mill to obtain the Cu-Ni-Si green sheet; this embodiment controls The gap between the rolls is such that the thickness of the Cu-Ni-Si green sheet is 0.3mm.

Step 3, atmosphere sintering

First put hydrogen into the atmosphere furnace, raise the temperature of the Cu-Ni-Si green sheet to 700°C for sintering in a hydrogen atmosphere, then put argon into the furnace body, raise the temperature to 900°C under an argon atmosphere for sintering for 1 hour, Finally, when the temperature of the furnace body drops to room temperature, the Cu-Ni-Si alloy plate is obtained.

Example 5

The direct powder rolling method for the rapid preparation of Cu-Ni-Si alloy sheet provided in this embodiment comprises the following steps:

Step 1, Mixing

Weigh 90g electrolytic Cu elemental powder (purity above 99.9%, average particle size 20um), 8g pure Ni powder (purity above 99.9%, average particle size 1um), 2g single crystal Si powder (purity above 99.9%, average particle size 1um ) and mixed to obtain Cu-Ni-Si mixed powder; in this embodiment, first pure electrolytic Cu elemental powder is added in the powder mixer, and then vacuum pump oil and ZrO of 0.8% electrolytic Cu mass are added Balls ₍ the ratio of ball to material is 1:4) were mixed for 1 h, then Ni powder and single crystal Si powder were added and mixed for 2 h. In this step, it is only necessary to mix the three raw materials evenly, and the mixing method and mixing tools are not limited.

Step 2, Rolling

Put the Cu-Ni-Si mixed powder into the powder rolling mill for secondary rolling, and control the gap between the rolls by adjusting the fine screw on the rolling mill to obtain the Cu-Ni-Si green sheet; this embodiment controls The gap between the rolls is such that the thickness of the Cu-Ni-Si green sheet is 0.3mm.

Step 3, atmosphere sintering

First put hydrogen into the atmosphere furnace, raise the temperature of the Cu-Ni-Si green sheet to 700°C for sintering in a hydrogen atmosphere, then put argon into the furnace body, raise the temperature to 950°C for sintering in an argon atmosphere for 1.1h , and finally when the temperature of the furnace body drops to room temperature, the Cu-Ni-Si alloy plate is obtained.

Fig. 2 (a) is the SEM image of the gas-atomized Cu powder used in Example 1, and Fig. 2 (b) is the SEM image of the electrolytic Cu powder used in Embodiment 2-5, as can be seen from it, the gas-atomized Cu powder The shape of the electrolytic Cu powder is spherical, while the shape of the electrolytic Cu powder is irregular, and most of them are distributed in dendritic accumulation. Compared with the gas-atomized Cu powder, the electrolytic Cu powder is easier to be rolled and formed, and the formability is better. Therefore, the present invention Choose electrolytic Cu powder.

Figure 3(a) is the macroscopic image of the Cu-Ni-Si green plate after two-pass rolling in Example 4, Figure 3(b) and Figure 3(c) are the images of Example 2 and Example 3 respectively Macroscopic image of Cu-Ni-Si green sheet after three-pass rolling. It can be clearly seen from Figure 3 that after the second rolling pass, the metal plate has good toughness and is not easy to break, and its length can reach about 95 mm; after the third rolling pass, the edge of the plate curls (Figure 3b The circled part) and cracking (the boxed part in Figure 3c) seriously affect the comprehensive performance of the plate. Therefore, the present invention prefers two passes of rolling.

Figure 4 is an image of the microstructure of the sintered Cu-Ni-Si alloy plate of Example 4 at 900 ° C. It can be seen from the figure that there are some tiny cavities (the part circled by the box) on the surface of the microstructure, and the copper powder particles The connection is not tight.

Figure 5(a) and Figure 5(b) are the microstructure images of the sintered Cu-Ni-Si alloy plate in Example 5 at 950 °C. It can be seen from the figure that the surface of the plate microstructure after sintering at 950 °C is not Larger voids or defects appear, and the Cu-Ni-Si mixed powder is more tightly combined.

Fig. 6 (a) is the elongation-tensile strength figure of pure copper sheet material, and Fig. 6 (b) is the elongation rate-tensile strength figure of the prepared Cu-Ni-Si alloy plate material of the present invention, from the figure It can be seen that compared with the pure copper sheet, the tensile strength of the Cu-Ni-Si alloy sheet is increased by 2.5 times.

Claims (6)

1. quickly preparing the direct powder rolling method of Cu-Ni-Si latten, which comprises the following steps:

Step 1, mixing

It weighs Cu, Ni, Si powder to be mixed, obtains Cu-Ni-Si mixed-powder；

Step 2, it rolls

The Cu-Ni-Si mixed-powder is rolled, Cu-Ni-Si green compact plate is obtained；

Step 3, atmosphere sintering

The Cu-Ni-Si green compact plate is sintered in a hydrogen atmosphere first, is then sintered under an argon atmosphere, finally to furnace body Temperature is down to room temperature to get the Cu-Ni-Si sheet alloy.

2. the direct powder rolling method as described in claim 1 for quickly preparing Cu-Ni-Si latten, which is characterized in that In the step 1, Cu powder is electrolysis Cu powder, and Si powder is single crystalline Si powder.

3. the direct powder rolling method as described in claim 1 for quickly preparing Cu-Ni-Si latten, which is characterized in that In the step 1, weighed Cu powder average particle size is 1um for the average grain diameter of 20um, Ni powder and Si powder.

4. the quick direct powder rolling method for preparing Cu-Ni-Si latten as described in any one of claims 1-3, It is characterized in that, in the step 1, according to mass percent meter, weighed Ni powder accounts for the 7%- of Cu-Ni-Si mixed-powder 8%, Si powder accounts for the 1.5%-2% of Cu-Ni-Si mixed-powder, remaining is Cu powder, the sum of mass percent of above-mentioned raw materials It is 100%.

5. the direct powder rolling method as described in claim 1 for quickly preparing Cu-Ni-Si latten, which is characterized in that In the step 2, the rolling of two to three passages is carried out to the Cu-Ni-Si mixed-powder using powder rolling machine.

6. the direct powder rolling method as described in claim 1 for quickly preparing Cu-Ni-Si latten, which is characterized in that In the step 3, sintering temperature is 680 DEG C -720 DEG C in a hydrogen atmosphere, and sintering temperature is 900 DEG C -980 under an argon atmosphere DEG C, sintering time 1h-1.5h.