CN1290655C - Preparation method of low oxygen content microballon parent metal powder and its special equipment - Google Patents

Abstract

The present invention relates to a powder preparation method, particularly to a preparation method of low oxygen content micro-ballon solder powder and a special equipment of the method. The preparation method has the procedures as following: base material of solder (such as Pb group, Sn group, Sn-Zn group, Ag group or Cu group) after heated and melted filling into an atomizer rotating at a high speed stably to carry out centrifugal atomization; the rotary speed of the atomizer is 4000 to 40000 revolutions per minute; melt objects obtain a high speed rotation energy atomizing the edge of the atomizer to form micro liquid drops which coagulate as spherical powder by surface tension in flight. The special device comprises a melting package arranged in a closed type atomizing container, an atomizer, a thermostat and a motor for driving the atomizer to rotate. The present invention is easy to prepare 15 to 104 mu m of micro spherical powder, the size of the powder has narrow distribution, high rate of finished products and better sphericity. An atomizing chamber is vacuated or filled with noble gases of N2, Ar, etc. to avoid powder oxidation; the oxygen content is less than 100 ppm.

Description

A kind of preparation method and special equipment thereof of low oxygen content microballoon solder powder

Technical field

The present invention relates to the powder preparation technology, be specially a kind of preparation method and special equipment thereof of low oxygen content microballoon solder powder.

Background technology

Current many electronic and electrical equipments such as notebook computer, mobile phone, video cameras etc. all adopt soldering paste welding printed circuit board (PCB), main component in the soldering paste is alloy system solder powders such as Pb-Sn, Sn-Zn-Bi and Sn-Ag-Cu, three main technical requirements to this powder are: fine size, generally need＜200 orders, μ m promptly＜74, many occasions need 325 orders, i.e. 44 μ m powder; Be shaped as sphere; Oxygen content less than 100ppm to guarantee welding quality.The main at present inert gas atomizer manufactured that adopts, being about to alloy melting flows out, with gases at high pressure it is sprayed into drop and condenses into powder, the subject matter that this method exists is that the size distribution of gained powder is very wide, yield rate is lower, and because of interference in air flow, the sphericity of powder is relatively poor, and oxygen content is often more than 150ppm, thereby the cost of this method is higher.

Chinese invention patent application (application number 00104536.9) discloses the preparation method and the device of a kind of noble metal and alloy powder thereof, by custom-designed device the supersonic gas atomizing is combined into a comprehensive powder by atomization step with centrifugal one-level circular cone atomizing and three grades of atomizings of circle drum of relative rotation at a high speed, selects corresponding technological parameter to prepare noble metal and alloy superfines thereof.

Chinese invention patent application (application number 94114891.2) discloses a kind of producing method for superfine homogeneous aluminium powder; the disc-type atomiser of the high speed rotation of aluminium liquid in closed container carries out powder by atomization; blanketing with inert gas simultaneously and convey materials; solid and gas through separator separates, and obtains the superfine aluminium power of oil immersion.

The weak point of above-mentioned two pieces of documents is: be difficult to obtain that size distribution is more even, the better powder of sphericity, and directly classification goes out the powder of different brackets granularity.

Summary of the invention

The object of the present invention is to provide a kind of preparation method and special equipment thereof of low oxygen content microballoon solder powder, make the narrower particle size distribution of powder, sphericity better, thus the yield rate height.

Technical scheme of the present invention is to make its degree of superheat reach 30～300 ℃ after the scolder raw material heat fused, to stablize the interior centrifugal atomizing of atomizer that flow velocity (flow rates is 3～50 Grams Per Seconds) injects rotation at a high speed, the atomizer diameter is φ 30～100mm, the atomizer rotating speed is 4000～40000 rev/mins, make it obtain the high speed rotation function, be fine droplets in the atomizing of atomizer edge, in flight course, be condensed into spherical powder because of surface tension, the granularity of powder is 15～104 μ m, and its oxygen content is less than 100ppm.

Described atomizer rotating speed is preferably 8000～18000 rev/mins; Described scolder can be one of Pb base, Sn base, Sn-Zu base, Cu base and Ag base; Described centrifugal atomizing can carry out in a vacuum, and vacuum is 5～5 * 10 ^-2Described centrifugal atomizing is at Ar, N ₂, carry out in He or the air, pressure is 0.01～0.2MPa.

Special equipment of the present invention comprises fusing bag, atomizer, the thermostat that places in the closed atomizing container and drives the motor that atomizer rotates, wherein atomizer is positioned at fusing bag below, revolution container for upper end open, thermostat is installed on the atomizer bottom, the outside of turning cylinder is covered with the water cooling chamber, motor places in the water cooling chamber, and the atomizing container bottom is connected with powder-collecting chamber.

Described atomizer diameter is φ 30～100mm; Described motor is with the coaxial high-speed electric expreess locomotive of atomizer or by the bel-drivenn high-speed electric expreess locomotive.

In order to realize high-revolving requirement, the present invention can adopt high stability dynamic balancing rotary device and high-precision high-speed bearing, guarantee high-speed balancing, and adopt the strong graphite of superelevation, BN, light metal Al, Ti or stainless steel material to make high-efficiency atomizer, the huge centrifugal force that makes it can bear high rotating speed and produce, making melt effectively obtain rotating in atomizer again can; Adopt radiator valve to make atomizer maintenance constant temperature in the atomization process, prevent melt solidifying or overheated.

One of principle of the present invention is the surface energy that melt high speed rotation function is converted into powder.When melt during in centrifugal rotation, its energy of rotation is mR ²ω ²/ 2, atomizing is powder, and when flight, and its surface can be 3 γ m/r ρ, and flight kinetic energy is mv ₀ ²/ 2, wherein m is a drop mass, and R is a radius of turn, and ω is an angular velocity of rotation, and γ is a surface tension, and ρ is a drop density, and r is a droplet radius, v ₀Be molten drop flight initial velocity.Its energy relationship is: mR ²ω ²/ 2=3 γ m/r ρ+mv ₀ ²/ 2

Because the surface can be inversely proportional to liquid-drop diameter by item, the surface of fine powder can be very high, in order to prepare fine powder, should make the liquid at high speed rotation, to obtain high as far as possible rotation function, be converted into the surface energy of small droplet simultaneously effectively at the atomizer edge, thus the flight initial velocity v of restricting liquid drop ₀, can reduce container diameter.

Two of the principle of the invention is the flight of control powder, thereby realizes the classification of powder.The spherolite that when diameter is d is with initial velocity v ₀When flying in density is the medium of ρ, under gravitational field g effect, the differential equation of motion of its level and vertical direction is respectively:

$\frac{\mathrm{dv}}{\mathrm{dt}}=-\frac{6}{\mathrm{\π}}\frac{{\mathrm{cvv}}_x}{d}\frac{\mathrm{\ρ}}{{\mathrm{\ρ}}_s}$

$\frac{{\mathrm{dv}}_y}{\mathrm{dt}}=g\frac{\mathrm{\ρ}-{\mathrm{\ρ}}_s}{{\mathrm{\ρ}}_s}-\frac{6}{\mathrm{\π}}\frac{{\mathrm{cvv}}_y}{d}\frac{\mathrm{\ρ}}{{\mathrm{\ρ}}_s}$

Wherein c is a resistance coefficient; V is a flying speed; V _x, v _yBe the flying speed component; ρ _sBe spherolite density; T is the time.

The different grain size powder has different tracks, and as change of flight initial velocity v ₀And pressure medium is when being density p, and flight path changes, thereby can realize the classification of powder size.

The invention has the beneficial effects as follows:

1. the present invention injects the atomizer centrifugal atomizing with the scolder heat fused, when increasing rotational energy, when particularly improving velocity of rotation, reach 10000～40000 rev/mins as rotating speed, be that ω reaches 1047～4188 radian per seconds, the ratio of its normal acceleration/acceleration of gravity reaches 4.5 * 10 ⁴2.5 * 10 ⁴Doubly, can obtain fabulous atomizing effect, the powder size distribution is very narrow, yield rate is high, sphericity is better, is easy to produce the minute spherical powder about 15～104 μ m.

2. adopt closed inflation atomizer, fill Ar, the N of 0.01～0.2MPa ₂, inert gas or air such as He, both can prevent the powder oxidation because of rapid solidification, controlled again powder process end flight is convenient to grading and is reclaimed, oxygen content is low in the powder, can reach below the 100ppm.

3. production cost is low.

Description of drawings

Fig. 1 is a special equipment structural representation of the present invention.

Fig. 2 is another example structure schematic diagram of special equipment of the present invention.

The specific embodiment

Embodiment 1

Preparation Pb-Sn alloy medium size powder (74～104 μ m) in the air:

As shown in Figure 1, the special equipment of present embodiment, comprise fusing bag (crucible) 1, atomizer 2, thermostat 3, the bearing 4 that places in the closed atomizing container 9 and drive the motor 5 that atomizer rotates, wherein atomizer 2 is positioned at fusing bag 1 below, is the revolution container of upper end open, and thermostat 3 is installed on atomizer 2 bottoms, bearing is installed on the atomizer turning cylinder, the outside of turning cylinder is covered with water cooling chamber 6, and motor 5 places in the water cooling chamber 6, and atomizing container 9 bottoms are connected with powder-collecting chamber 7; The atomizer diameter is φ 50mm, and motor 5 is for passing through the bel-drivenn high-speed electric expreess locomotive.

Get 2 kilograms of Pb-61.9%Sn alloys, in band is let slip a remark 8 crucible, be heated to 250 ℃, make its fusing, φ 50mm atomizer is preheated to 250 ℃, by motor its drive is gone to 8000 rev/mins, discharge spout 8 place's stoppers are opened, and liquation is by 8 outflows of leting slip a remark, and flow velocity is 5 Grams Per Seconds, its flows into behind rotary atomizer by centrifugal atomizing, condensing at flight course becomes spherical powder, and particle size range is 74～104 μ m, and the oxygen content of powder is 90ppm.

Embodiment 2

Preparation Pb-Sn alloy fine granularity powder (44～74 μ m) in closed container, difference from Example 1 is: as shown in Figure 2, the atomizer diameter is φ 60mm, and motor 5 is the high-speed electric expreess locomotive coaxial with atomizer.

In closed container, charge into the 0.1MPa high pure nitrogen, the oxygen content of its gas is less than 100ppm, 20 kilograms of Pb-61.9%Sn alloys are heated to 300 ℃ of fusings, is that the atomizer of φ 60mm accelerates to 10000 rev/mins with coaxial high-speed electric expreess locomotive with diameter, the flow velocity of opening control melt behind the stopper is the 15-25 Grams Per Second, and gained spherical powder particle size range is 44～74 μ m, and the oxygen content of powder is 80ppm.

Embodiment 3

In closed container, prepare very fine granularity powder (30～50 μ m) of Pb-Sn alloy, difference from Example 2 is: in closed container, charge into the 0.09MPa high-purity argon gas, the oxygen content of its gas is less than 100ppm, 20 kilograms of Pb-61.9%Sn alloys are heated to 320 ℃ of fusings, is that the atomizer of φ 60mm accelerates to 12000 rev/mins with coaxial high-speed electric expreess locomotive with diameter, the flow velocity of opening control melt behind the stopper is 10～15 Grams Per Seconds, gained spherical powder particle size range is 30～50 μ m, and the oxygen content of powder is 85ppm.

Embodiment 4

Difference from Example 2 is: in closed container, charge into the 0.05MPa high-purity argon gas, the oxygen content of its gas is less than 100ppm, 20 kilograms of Pb-61.9%Sn alloys are heated to 370 ℃ of fusings, is that the atomizer of φ 80mm accelerates to 18000 rev/mins with coaxial high-speed electric expreess locomotive with diameter, the flow velocity of opening control melt behind the stopper is 10～15 Grams Per Seconds, and gained spherical powder particle size range is 15～50 μ m, and the oxygen content of powder is 70ppm.

Embodiment 5

Difference from Example 2 is: in closed container, charge into the 0.05MPa high-purity argon gas, the oxygen content of its gas is less than 100ppm, 20 kilograms of Sn-8Zn-3Bi alloys are heated to 400 ℃ of fusings, is that the atomizer of φ 60mm accelerates to 12000 rev/mins with coaxial high-speed electric expreess locomotive with diameter, the flow velocity of opening control melt behind the stopper is 10～15 Grams Per Seconds, and gained spherical powder particle size range is 30～50 μ m, and the oxygen content of powder is 75ppm.

Claims (6)

1. the preparation method of a microballoon solder powder, adopt centrifugal atomizing, scolder is the Sn base, the Pb base, one of Sn-Zn base and Cu base, it is characterized in that: will carry out centrifugal atomizing to stablize in the atomizer that flow velocity injects rotation at a high speed after the scolder raw material heat fused, the degree of superheat of described heat fused reaches 30～300 ℃, described flow rates is 3～50 Grams Per Seconds, described atomizer diameter is φ 30～100mm, the atomizer rotating speed is 10000～40000 rev/mins, make melt obtain the high speed rotation function, be fine droplets in the atomizing of atomizer edge, drop is condensed into low oxygen content microballoon scolder spherical powder because of surface tension in flight course, the granularity of powder is 15-104 μ m, and its oxygen content is less than 100ppm.

2. according to the preparation method of the described microballoon solder powder of claim 1, it is characterized in that: described centrifugal atomizing carries out in a vacuum, and vacuum is 5～5 * 10 ^-2Pa; Perhaps at Ar, N ₂, carry out in He or the air, pressure is 0.01～0.2MPa.

3. according to the preparation method of the described microballoon solder powder of claim 1, it is characterized in that: described atomizer rotating speed is 8000～18000 rev/mins.

4. special equipment according to the preparation method of the described microballoon solder powder of claim 1, adopt centrifugal atomizer and atomizing container, it is characterized in that: comprise the fusing bag (1) that places in the closed atomizing container (9), atomizer (2), thermostat (3) and the motor (5) that drives the atomizer rotation, wherein atomizer (2) is positioned at fusing bag (1) below, revolution container for upper end open, thermostat (3) is installed on atomizer (2) bottom, the outside of turning cylinder is covered with water cooling chamber (6), motor (5) places in the water cooling chamber (6), and atomizing container (9) bottom is connected with powder-collecting chamber (7); Described atomizer (2) diameter is φ 30～100mm.

5. according to the described special equipment of claim 4, it is characterized in that: described motor (5) is for the coaxial high-speed electric expreess locomotive of atomizer (2) or by the bel-drivenn high-speed electric expreess locomotive.

6. according to the described special equipment of claim 4, it is characterized in that: described atomizer (2) adopts graphite, BN, light metal Al, Ti or stainless steel material to make.

Images