JPS6067594A - Solid lubricant - Google Patents

Abstract

PURPOSE:A solid lubricant consisting essentially of a specific graphite fluoride obtained by reacting a crystal graphite with a specific ash content with fluorine, and capable of reducing the wear of metal. CONSTITUTION:A solid lubricant consisting essentially of graphite fluoride of the formula (C2F)n obtained by fluorinating natural or artificial crystal graphite with <=3wt% ash content under 700mm.Hg fluorine pressure at 375 deg.C for 50hr. The above-mentioned graphite fluroide obtained by crystallizing the graphite fluoride after completing the reaction at a higher temperature than the formation temperature has the similar improved characteristics.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention provides graphite fluoride (hereinafter referred to as I) used in solid lubricants.
+ (represented by 3Fll) and aims to provide a solid lubricant that provides excellent lubricity.

OF is a solid powder that has unique lubricity, water and oil repellency, and excellent chemical resistance, so it is used as a solid lubricant, anti-filtering agent, antifouling agent, water and oil repellent, etc. ing.

On the other hand, it is well known that it is useful as a battery active material and provides a high energy density primary battery tube with good battery storage stability. As described above, OF is highly evaluated industrially in a wide range of fields, and is a compound that can be expected to be applied and developed in many more fields in the future.

One type of OF is polymonocarbon monofluoride represented by (OF)n, which is well known to be useful as a battery active material as mentioned above (4!
! (Refer to the specification of F. Publication No. 48-25565). (OF)n
is reacted with an amorphous carbon material such as petroleum coke at a temperature of about 2000 to about 450°C, or
It is obtained by reacting a crystalline carbon material such as natural or artificial graphite with fluorine at a temperature of about 00°C to about 650°C. Yet another (IF) was discovered by Tsuyoshi Watanabe (01
B') There is a polycarbonate monofluoride represented by n. (OIF)n can be obtained in relatively high yield and at low cost. As detailed in JP-A-55-102895 and US Reissue Patent No. Re30667, graphite material f100-760ml
It is obtained by heating at 500-500°C under a fluorine pressure of 1Hg. As the graphite material used for manufacturing (0@F)n, natural graphite, artificial graphite, quiche graphite, pyrolytic graphite, or a mixture thereof can be used. It has a laminated structure in which layers forming an (4F)n-scale lattice structure are stacked with an interlayer distance of 9.0×, and is different from the crystal structure of (OF)n, which has an interlayer distance of about 6×. Also, each carbon in each layer is (OF)
In the case of n, each is bonded to one fluorine atom, whereas
In the case of (0!F)n, every other carbon in each layer is bonded to one fluorine. However, 0F)n and (011P
)n, there are OF, group and GF1 group as peripheral groups at the ends of the carbon hexagonal network layer of the compound. Therefore, if graphite is completely fluorinated, (OF)n and (
o, p)n (7) The F/C ratio is each k O,5 or more and 1.0 or more. The amount of excess fluorine caused by surrounding OIF and GF1 group increases as the size of the crystal in the al-b axis direction of the GF crystal becomes smaller [Journal of
American Chemical Society, Volume 101.

5852 pages 19791f-(J, Amer, Ohem,
8oc, IOI, 5832 (see September 197).As can be seen from the above, depending on the reaction conditions and the crystallinity or type of carbon material, (op)n, (OF)n, or a mixture thereof can be obtained. , it is also possible to leave all unreacted carbon material in these GFs.

As is clear from the above, the composition and structure of GF produced by fluorination of a carbon material depend on the reaction temperature and the type or crystallinity of the carbon material. On the other hand, the physical properties of the produced GF are also considered to strongly depend on the type and characteristics of the carbon material to be fluorinated. However, when using G'Ff as a solid lubricant containing (OtF)nf as its main component, no detailed study has been made regarding the raw material carbon.

The present inventors conducted a detailed study on crystalline graphite, such as natural graphite and artificial graphite, used as raw materials for the production of (OIF)n. The lubricating properties of OF containing n' as the main component are different, and it has been found that fluorinated crystalline graphite with an ash content of 5F% or less has excellent lubricating properties, and the present invention has been completed.

That is, as a raw material for (01F')n type ay, the ash content is 5.
It has been found that when (OIF)n obtained by fluorinating crystalline graphite with F% or less is used as a solid lubricant, a low wear rate is exhibited.

The GF mainly composed of ((4F)n?) according to the present invention, which is crystallized at a high temperature higher than the formation temperature in a zero fluorine atmosphere after the completion of the reaction, also has excellent properties. The lubricants can be applied in a variety of forms, either alone or in combination with other lubricants.

The present invention will be explained in more detail below with reference to Examples, but the scope of the present invention is not limited to the Examples.

The lubricating properties of Examples and Comparative Examples were determined by the following method.

OF3. Op'e, along with 100 iron balls with a diameter of 120, were placed in a bot mill (inner diameter: 70 m, length: 8 (m)) and rotated.Then, the iron balls were taken out, and the total amount of wear was measured from the weight of the iron balls.

5- Example Summer-5 Ash content, 0.5W arc2. OW Qi and 3. OW's natural graphite (average particle 10.um)'i fluorine material 00m+ll
Fluorination reaction was carried out at 575°C for 50 hours under Hg (0
2F) OF whose main component is n? Obtained.

The obtained ay/c ratios are all 0.62, and the X-ray diffraction diagram has a diffraction line with a peak at 2θ-10.0°.
In addition, it shows infrared absorption at 940I:fn, and (0!F
) was proven to be n-type GF.

The lubricating properties of the obtained GF were measured by the method described above.

The results are shown in Table 1.

Example 4 Artificial graphite (average particles = 6) with an ash content of 0.5 F% was subjected to a 4-fluorination reaction under 700 μHg at '□375°C to produce (0*F')n' GFft with f principal component
Obtained.

The F2O ratio of the obtained GF was 0.68, and the X-ray diffraction diagram had a diffraction line with a peak t at 2θ-10. It was proven to be type GF.

6- The lubricating properties of the obtained OF were measured in the same manner as in Example 1.

The results are shown in the summer table.

Comparative Example 1-2 Ash content 4. OW%, 10W% natural graphite (average particles, 1
0μm) under a fluorine pressure of 700wttBg, 375
A fluorination reaction was carried out at ℃ for 50 hours to obtain OF containing (0!F)nt as a main component.

The y10 ratios of the obtained GFs were all 062, and the X-ray diffraction diagram had a peak at 2θ-10,0°, and also showed infrared absorption at 94o, indicating (01'F) n-type. G
'fP.

The lubricating properties of the obtained GF were measured in the same manner as in Example 1.

The results are shown in Table 1.

Comparative Example 5 Artificial graphite with ash content s, owl (average particle size 1 μm) 7i
c-Fluorine treatment 700+a+Hg at 560℃ for 50
A fluorination reaction was carried out for a period of time to obtain GF containing (01P)n'fr as a main component.

The φ ratio of the obtained GF was 0.70, and the X-ray diffraction pattern showed 2
There is a diffraction line with a peak number at θ-Io, 4°, and 9
40. It showed infrared absorption, and was proved to be an (OIF)n-type GF.

The lubricating properties of the obtained OF were measured in the same manner as those of the examples. The results are shown in Table 1.

As is clear from Table 1 and above, crystalline graphite with an ash content of 5 w% or less is used as a raw material. : It can be seen that when (0*F)n is used as a lubricant, the amount of metal wear is small.

Patent applicant: Central Glass Co., Ltd. 9-

Claims (1)

[Claims] A solid lubricant whose main component is fluorinated graphite expressed by the formula (01IF)n obtained by reacting crystalline graphite with an ash content of 5 W% or less with fluorine.