JPS60112639A - Bushing for forming fiber - Google Patents

Abstract

PURPOSE:To obtain fins for cooling having durability and causing no brittle rupture when bushing for forming inorg. fibers is manufactured, by coating Ag fins for cooling with Pd or a Pd alloy so as to form a composite material. CONSTITUTION:Plural nozzles 2 are projected in lines from the bottom plate of the body 1 of a vessel for storing a starting material for fibers, and fins 3 for cooling connected to a pipe 4 for water cooling are placed among the lines of the nozzles 2 without bringing the fins 3 into contact with the nozzles 2 and the body 1. A round Ag bar is fixed in a Pd or Pd alloy pipe, and diffusion treatment is carried out in gaseous N2 so as to form a diffusion layer of >=3mum thickness between Ag and Pd and to leave a Pd layer of >=about 2mum thickness. The Ag bar and the Pd pipe united to one body are plastically worked to a prescribed shape and subjected to strain relief annealing. The fins 3 are made of the resulting composite material. The fins 3 for cooling do not cause warping deformation due to the difference in coefft. of thermal expansion between Ag as the core material and Pd as the shell material.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a fiber-forming bushing used for spinning inorganic fiber raw materials such as molten glass by discharging them from a number of nozzles.

The kR fiber forming bushing is made of Pt or Pt alloy and contains the melted fiber raw material, and usually has a structure as shown in FIGS. 1 to 4. Figure 1 is an overall side view showing the spinning state, Figure 2 is a partial perspective view from the bottom of the fiber forming bushing, Figure 3 is a partial bottom view, and Figure 4 is a part showing the state of the nozzle and cooling fins. This is an enlarged view. In the figure, 1 is the main body of the storage container for the truncated rectangular ↑li [H-shaped fiber raw material, and 2 is the nozzle 3 protruding from the bottom plate of the storage container main body 1 is the inorganic material discharged from the nozzle 2. These cooling fins cool the fibers, and are arranged between 20 rows of nozzles so as not to touch the nozzles 2 and the storage container body 1, as shown in Fig. 3.Ag is used as a material with good thermal conductivity. ing. 4 is a water cooling pipe that cools the cooling fins 3; this water cooling pipe 4 cools the cooling fins 3;
are consecutive. A heating electrode 5 keeps the fiber raw material in the storage container body 1 at a temperature in a molten state.

6 is an inorganic fiber, and 7 is a fiber sleeping device.

Inorganic fibers are spun using the fiber-forming bushing described above, but the tolerance for the diameter (fC) of spun inorganic fibers has traditionally been very small, especially with the recent development of the electronic industry. Demand for inorganic fibers has increased rapidly, and in terms of quality, high dimensional accuracy such as diameter has become required.

Therefore, in order to meet the above-mentioned high accuracy, the composition of the raw material, the electrical conditions for current heating, the mechanical precision of the fiber-forming bushing, the mounting condition when combined with refractory materials, etc., the holding temperature of the molten raw material, etc. These are the conditions for maintaining the appropriate viscosity of the bath-fiber raw material when it is discharged from the nozzle.

Therefore, cooling fins 3 have been conventionally disposed in order to stably and continuously discharge extremely fine inorganic fibers from the nozzle.

This cold prisoner fin 3 surrounds the discharge unit D [to protect it from external influences such as wind and dust, and also to instantaneously cool the nozzle 2 and the inorganic fibers being discharged. As mentioned above, Ag, which has the best thermal conductivity among metals, is generally used. By connecting these cooling fins 3' (IL--to the water cooling vibe 4), heat near the nozzle is efficiently absorbed.

When inorganic fibers are made into molten glass, the temperature is generally 1
Since the temperature is maintained at about 200° C. to 1400° C., the temperature of the cooling fins 3 disposed close to the nozzle 2 is also exposed to a considerably high temperature.

Figure 5 shows the thickness 1 and 2 after 140 hours have passed since installation.
This is a photograph showing the +Qr plane composition of a cooling fin made of Ag for RAM, and the two crystal grains have grown to a size of 1 approximately equal to the thickness. This also shows how the cooling fins are exposed to high temperatures.

! CLI also has excellent heat conductivity and is inexpensive, but oxidation is severe at high temperatures and a sufficient cooling effect in the vicinity of the nozzle cannot be expected. Therefore, Ag is used as the material for the cooling fins, but as is well known, Ag easily forms compounds with sulfur. It is attacked by even the smallest amount of sulfur present in the atmosphere. Therefore, a considerable amount of yellowish content present in the raw material of bath molten glass has a large adverse effect on the cooling fins.

The sulfuric gas generated from the semi-molten glass fibers discharged from the nozzle reacts extremely easily with the Ag cooling fins maintained at high temperatures, producing sulfuric Ag f mainly at the grain boundaries. Put it away.

As time passes, this progresses from the surface toward the inside and becomes brittle, causing layer-like chipping and wear.

Such defects inside the cooling fins due to Ag sulfide are
In addition to lowering the thermal conductivity, the volume reduction due to chipping and wear significantly lowers the cooling efficiency, making it impossible to obtain normal glass fibers.

In addition, when the cooling fins (Ag) come into contact with the surface of the pi- or pt gold alloy fiber-forming bushing held at high temperature, the Ag rapidly leaks into the grain boundaries of the PL-j or Pi alloy, causing a certain stress. Imp! Causes IE destruction. That is, since the cooling fins are disposed close to the fiber forming bushing and the nozzle, the above-mentioned accident occurs due to movement of the cooling fins.

The causes of this movement of the cooling fins are as follows. The first is direct contact with cooling fins due to deformation due to the weight of the molten raw material in the fiber-forming bushing;
The second is the accumulation of localized Ag by contact with the discharged inorganic fibers and cooling fins, and the third is the gradual buildup of Ag sulfide. l! There are natural deposits of Ag (such as ★), but there are currently no definitive city prevention measures against them.

Furthermore, the emissivity of Ag is one of the smallest elements among metals, and therefore it tends to reflect heat from the vicinity of the nozzle, resulting in very poor cooling efficiency.

Therefore, it is conceivable to replace Ag with an element that has a higher thermal emissivity than Ag and is more resistant to sulfidation, and which does not have a significant adverse effect even when it comes into contact with Pt or PL alloy.

These elements include Au and Pd.

There are P [+ W+ +p i + Zr lN 1, etc. However, it was found that Ni, W, Ti, and Zr (or 4 metals) could not be used for a single period of time because their oxidation resistance at elevated temperatures was extremely poor.

Therefore, the present invention aims to solve the above-mentioned drawbacks [1]
9, and the above drawbacks are solved by combing with Ag i Pd or Pd alloy.A pipe is made of Pd or Pd alloy, and a hole is inserted into the pipe.
& is combined and subjected to diffusion treatment in N2 gas to form a diffusion layer of 3μ or more between Ag and Pd or Pd alloy, and Pd
Or [/I of Pd alloy! #' is formed to have a thickness of 2μ or more and is integrated, so that it can be used as a cooling fin with a large temperature gradient, and it can be used as a cooling fin with a large temperature gradient. The cooling fin is characterized by eliminating deformation, being durable, and free from brittle fracture.

The present invention will be explained in detail below.

1st laugh 7If! 1 exception diameter φ], 5 am, inner diameter φ14.11+111.
A Pd pipe with a length of 500 am and a diameter of 14.35 mm.
, insert and fit an Ag round bar with a length of 700 ram, and
The PC+ pipe and Ag round bar are brought into close contact by drawing with a round die having a diameter of 9 rhymes to form a composite material.

This closely adhered composite material was preheated by heating at 900° C. for 2 hours in N2 gas. Next, it was drawn again using a die with a diameter of 14.8 mm and heated at 920°C in N2 gas for 2 hours.
A time diffusion process was performed.

After that, roll the ribbon to a thickness of 1.2 mm, medium 10
+s, cut to a length of 5Q'mm, and subjected to strain relief annealing at 600°C to produce cooling fins made of strip-shaped composite material.

According to this cooling fin made of a composite material of Pd and Ag, the circumferential surface of Ag, which has excellent thermal conductivity, has sulfidation resistance and
Pd, which has excellent brittleness resistance and heat absorption, is coated, and A-g and Pd0 are formed through a series of manufacturing processes: fitting → preliminary diffusion → plastic working → diffusion treatment → plastic working → strain relief annealing.
A diffusion j of 3μ or more is formed between them to form an integral structure.

The will and war that formed this diffusion layer will be described below.

At the end 1 of the cooling fin 3 in the opposite direction from the part where the joint τ with the cooling pipe 4 broke, and at the top E'1 of the cooling fin 3.
Since the temperature gradients at the valleys such as i3a and lower +flS3b are similar, if there is no diffusion layer at all, the thermal deformation caused by the slow rate of thermal expansion between Ag in the core and Pd in the outer skin will be large; It is not possible to extract inorganic fibers that meet strict dimensional specifications. The expansion rate of Fd is 18 degrees, half that of Ag, so if rapid diffusion treatment is performed, the composite material will lack uniformity, so the main diffusion treatment was performed after preliminary diffusion. Formation of a diffusion layer thus becomes an indispensable requirement.

Second implementation exception diameter φ15 dragon, inner diameter φ14.41 #lIn + length 500
'mtn 05Pd-, [r pipe diameter 1.4.3
5rx, length 700cm Ag circle (insert and fit fist, 1
95P is drawn using a round die with a diameter of 4.9mm.
(1-Ir pipe and Ag roundweed are brought into close contact to form a composite material.

This tightly adhered composite material was preheated by heating at 900° C. for 2 hours in N2 gas. Next, it was drawn again using a die with a diameter of 148 mm and heated at 920°C in N2 gas for 2 hours.
A time diffusion process was performed.

Then roll the ribbon to a thickness of 1.2 mm and a width of 10 mm.
A cooling fin made of a composite material in the shape of a short piece was created by cutting the piece to a length of 50 mm and annealing it at 600°C.

59 pd-Au, 30 Pd-R in a similar manner
Cooling fins were made from a composite material of t+ and 95Pd-Pt pipes and Ag round rods, and a mounting test was conducted.

As a result of the mounting test, as shown in the photograph of FIG. 6, the cooling fin made only of Ag had progressed to sulfurization and suffered from very severe chipping and wear, and was reduced to about half its initial thickness.

On the other hand, the cooling fins made of composite material remained in a healthy state without being attacked by corrosive substances such as yellowing, as shown in the photograph in FIG.

The usable alloy ratio of Pd alloy is Pd-1,r(0
,0i~30%) PdfL-Au (0,01~60
%), Pd-1Lu (,0,(l) ~20%
), Pd-1,lt (0.01-50%).

As described above, according to the present invention, Ag having excellent heat conductivity A9
The surrounding surface is covered with IJd or P (1 alloy), which has excellent sulfidation resistance, anti-4 brittleness, and heat absorption, and is coated with Ag and Pd.
Alternatively, by forming a composite material by forming (diffusion) ftt with a Pd alloy, a durable cooling fin can be obtained without reducing thermal conductivity.

[Brief explanation of the drawing]

Figure 1 is an overall side view showing the spinning state, Figure 2 is a partial perspective view from the bottom of the fiber forming bushing, Figure 3 is a partial bottom view, and Figure 4 is a part showing the state of the nozzle and cooling fins. An enlarged view, FIG. 51 is a photograph showing the cross-sectional structure of the Ag cooling fin, FIG. 6 is a photograph showing the state of wear and tear of the cooling fin due to Ag, and FIG. 7 is a photograph showing the cooling fin made of the composite material of the present invention. This is a photo showing the condition. 1...Storage container body 2...Nozzle 3...Cooling fin 4...Water cooling pipe Patent applicant Ajishiki Company Tokuriki Head Office Nittobo Co., Ltd. Agent Masuji Mikoto Kanakura 2 @ 1 voice

Claims (1)

[Claims] 1 A plurality of nozzles 20 are installed on the bottom plate of the fiber raw material storage container body.
In a fiber forming bushing in which cooling fins are protruded in rows and connected to a water cooling pipe between the nozzle rows so as not to touch the nozzles and the storage container body, the cooling fins are placed on the circumferential surface of Ag. l) A fiber-forming bushing characterized by using a composite material in which d or Pd liver metal is integrated by forming a diffusion Jli of 3μ or more, formed into a predetermined shape by plastic working, and then subjected to strain relief annealing.