阅读说明：本技术 一种耐热钢线材的表面草酸化润滑处理方法 (Surface straw acidification lubrication treatment method for heat-resistant steel wire ) 是由 刘平保 付星星 张宇 于 2021-06-30 设计创作，主要内容包括：本申请涉及金属材料加工领域,特别涉及一种耐热钢线材的表面草酸化润滑处理方法。本申请提供的耐热钢线材的表面草酸化润滑处理方法,包括以下步骤：S101,将固熔处理后的耐热钢线材浸泡在35-45℃的浸蚀活化剂中活化10-15min,活化结束后,清洗；S102,对清洗后的耐热钢线材进行第一次干燥；S103,将步骤S102第一次干燥后的耐热钢线材浸入65-70℃的草酸化转化剂中进行草酸化处理,草酸化处理结束后,清洗；S104,对步骤S103清洗后的耐热钢线材进行第二次干燥,之后置于室温中静置冷却,即得到表面覆盖有草酸化润滑膜的耐热钢线材。利用本申请提供的方法能够形成规则结晶的草酸化润滑膜,提升线材表面的润滑性能,有利于延长模具寿命和冷镦成型性能。(The application relates to the field of metal material processing, in particular to a surface straw acidification lubrication treatment method for a heat-resistant steel wire rod. The application provides a surface straw acidification lubricating treatment method of a heat-resistant steel wire rod, which comprises the following steps: s101, soaking the heat-resistant steel wire subjected to solid melting treatment in an etching activator at 35-45 ℃ for activation for 10-15min, and cleaning after the activation is finished; s102, drying the cleaned heat-resistant steel wire rod for the first time; s103, soaking the heat-resistant steel wire rod dried for the first time in the step S102 into an oxalic acid conversion agent at 65-70 ℃ for oxalic acid treatment, and cleaning after the oxalic acid treatment is finished; and S104, drying the heat-resistant steel wire rod cleaned in the step S103 for the second time, and then standing and cooling the heat-resistant steel wire rod at room temperature to obtain the heat-resistant steel wire rod with the surface covered with the oxalic acid lubrication film. By the method, the oxalic acid lubricating film with regular crystallization can be formed, the lubricating performance of the surface of the wire rod is improved, and the service life of the die and the cold heading forming performance are prolonged.)

1. A surface straw acidification lubrication treatment method of a heat-resistant steel wire rod is characterized by comprising the following steps:

s101, soaking the heat-resistant steel wire subjected to solid melting treatment in an etching activator at 35-45 ℃ for activation for 10-15min, and cleaning after the activation is finished;

s102, drying the cleaned heat-resistant steel wire rod for the first time;

s103, soaking the heat-resistant steel wire rod dried for the first time in the step S102 into an oxalic acid conversion agent at 65-70 ℃ for oxalic acid treatment, and cleaning after the oxalic acid treatment is finished;

and S104, drying the heat-resistant steel wire rod cleaned in the step S103 for the second time, and then standing and cooling the heat-resistant steel wire rod at room temperature to obtain the heat-resistant steel wire rod with the surface covered with the oxalic acid lubrication film.

2. The method for oxalation lubricating treatment of the surface of the heat-resistant steel wire rod according to claim 1, wherein in step S101, the etching activator comprises the following components in parts by mass: 20-25 parts of hydrochloric acid, 4-6 parts of sulfuric acid, 4-6 parts of nitric acid and 0.1-0.15 part of hexamethylenetetramine.

3. The method for carrying out the surface oxalation lubrication treatment on the heat-resistant steel wire rod as recited in claim 2, wherein in the step S101, the etching activator comprises the following components in parts by mass: 22 parts of hydrochloric acid, 5 parts of sulfuric acid, 5 parts of nitric acid and 0.13 part of hexamethylenetetramine.

4. The method for performing surface oxalation lubrication treatment on a heat-resistant steel wire rod according to claim 1, wherein in step S101, the heat-resistant steel wire rod has a chromium content of 13.5 wt% to 16 wt% and a nickel content of 24 wt% to 27 wt%.

5. The method for performing surface oxalation lubrication treatment on a heat-resistant steel wire rod according to claim 1, wherein the temperature for the primary drying in step S102 is 80-85 ℃.

6. The method for performing surface oxalic acid lubrication treatment on the heat-resistant steel wire rod according to claim 1, wherein in the step S103, the oxalic acid conversion agent comprises the following components in parts by mass: 36-38 parts of oxalic acid, 8-9 parts of ferric sulfate, 3-4 parts of sodium bisulfite and 1-1.5 parts of sodium thiosulfate.

7. The method for performing the surface oxalation lubrication treatment on the heat-resistant steel wire rod as claimed in claim 6, wherein in the step S103, the oxalic acid conversion agent comprises the following components in parts by mass: 37 parts of oxalic acid, 8.5 parts of ferric sulfate, 3.5 parts of sodium bisulfite and 1.3 parts of sodium thiosulfate.

8. The method for oxalation lubricating treatment of the surface of the heat-resistant steel wire rod according to claim 1, wherein the time for the oxalation treatment in step S103 is 25 to 30 min.

9. The method for performing surface oxalation lubrication treatment on a heat-resistant steel wire rod according to claim 1, wherein the temperature for the secondary drying is 80-85 ℃ in step S104.

10. The method for performing surface oxalation lubrication treatment on a heat-resistant steel wire rod according to claim 1, wherein the crystal size of the oxalation lubrication film is 4 to 12 μm.

Technical Field

The application relates to the field of metal material processing, in particular to a surface straw acidification lubrication treatment method for a heat-resistant steel wire rod.

Background

Fasteners are a class of mechanical parts that are used for fastening connections and are in wide use. The method has application in various machines, equipment, vehicles, ships, railways, bridges, buildings, structures, tools, instruments, supplies and the like. One common wire rod of the fastener is a cold heading steel wire rod, and because the lubricating requirement on the surface of the wire rod is higher in cold heading processing, the surface of the wire rod needs to be lubricated before cold drawing of the wire rod and cold heading forming of parts.

At present, lubricating processes adopted by manufacturers for steel wires are lubricating processes for common stainless steel wires such as SUS304 and SUS316, and the main process flows are three types: a. after wire material is solidified and melted, spraying pills → acid cleaning (25% sulfuric acid, temperature 60 ℃, time 1 hour) → water washing → acidification of grass (temperature 90 ℃, time 30min) → hot water washing → drying; b. shot blasting → acid cleaning (25% sulfuric acid, temperature 60 ℃, time 1 hour) → water washing → acidification of grass (temperature 90 ℃, time 30min) → hot water washing → drying before wire solid melting; c. acid washing (25% sulfuric acid, temperature 60 ℃, time 1 hour) → water washing → oxalic acid treatment (temperature 90 ℃, time 30min) → hot water washing → drying → dip coating of saponifier.

However, for the heat-resistant steel wire rod with high chromium content and nickel content, the following problems exist by using the lubricating process flow: 1) in the process flow, the sulfuric acid solution with higher concentration is used for soaking the material for a long time, so that excessive acid corrosion and hydrogen permeation can be caused to the material, and the performance of a subsequent bolt finished product is damaged; 2) because the contents of chromium and nickel in the heat-resistant steel are higher than those of common stainless steel, when the oxalic acid lubrication process of the common stainless steel is used for carrying out surface treatment on the heat-resistant steel, crystals with regular forms and complete coverage rate are difficult to form on the surface of a wire rod, and the two defects can cause the problems of galling on the surface of a part during cold heading forming, short service life of a die, even cracking of the head of the part and the like; 3) the oxalic acid technology temperature is required to be more than 90 ℃, the energy consumption is large and the oxalic acid technology temperature is not easy to guarantee; 4) the lubricating film formed on the surface of the wire rod by the prior art has short validity period, generally changes color when being stored for more than two to three months, and greatly reduces the lubricating property.

Therefore, it is necessary to provide a surface acidification lubrication treatment method for a heat-resistant steel wire rod.

Disclosure of Invention

The embodiment of the application provides a surface straw acidification lubrication treatment method for a heat-resistant steel wire rod, and aims to solve the problems of high energy consumption and low lubrication performance in the related technology by adopting wire rod lubrication processes of common stainless steel SUS304, SUS316 and the like.

In a first aspect, the present application provides a method for surface acidification and lubrication treatment of a heat-resistant steel wire rod, comprising the following steps:

step S101, soaking the heat-resistant steel wire subjected to solid melting treatment in an etching activator for activation, and cleaning after the activation is finished;

step S102, drying the cleaned heat-resistant steel wire rod for the first time;

step S103, soaking the heat-resistant steel wire rod dried for the first time in the step S102 into an oxalic acid conversion agent for oxalic acid treatment, and cleaning after the oxalic acid treatment is finished;

and step S104, drying the heat-resistant steel wire rod cleaned in the step S103 for the second time, and then standing and cooling the heat-resistant steel wire rod in room temperature to obtain the heat-resistant steel wire rod with the oxalic acid lubrication film covered on the surface.

In some embodiments, in step S101, the etching activator comprises the following components in parts by mass: 20-25 parts of hydrochloric acid, 4-6 parts of sulfuric acid, 4-6 parts of nitric acid and 0.1-0.15 part of hexamethylenetetramine.

In some embodiments, in step S101, the etching activator comprises the following components in parts by mass: 22 parts of hydrochloric acid, 5 parts of sulfuric acid, 5 parts of nitric acid and 0.13 part of hexamethylenetetramine.

In some embodiments, in step S101, the temperature of the etching activator is 35-45 deg.C and the activation time is 10-15 min.

In some embodiments, in step S101, the heat-resistant steel wire rod has a chromium content of 13.5 wt% to 16 wt% and a nickel content of 24 wt% to 27 wt%; the heat-resistant steel wire rod comprises the following components in percentage by mass: c is less than or equal to 0.08, Si is less than or equal to 1.0, Mn is less than or equal to 2.0, P is less than or equal to 0.025, S is less than or equal to 0.01, Mo: 1.0-1.5, Ti: 1.75-2.35, Al is less than or equal to 0.35, V: 0.1-0.5, B: 0.001-0.01, and the balance of Fe.

In some embodiments, the temperature of the first drying in step S102 is 80-85 ℃.

In some embodiments, in step S103, the oxalic acid conversion agent comprises the following components in parts by mass: 36-38 parts of oxalic acid, 8-9 parts of ferric sulfate, 3-4 parts of sodium bisulfite and 1-1.5 parts of sodium thiosulfate.

In some embodiments, in step S103, the oxalic acid conversion agent comprises the following components in parts by mass: 37 parts of oxalic acid, 8.5 parts of ferric sulfate, 3.5 parts of sodium bisulfite and 1.3 parts of sodium thiosulfate.

In some embodiments, in step S103, the temperature of the oxalic acid conversion agent is 65-70 ℃, and the time of oxalic acid conversion is 25-30 min.

In some embodiments, the temperature of the second drying in step S104 is 80-85 ℃.

In some embodiments, the oxalated lubricating film has a crystal size of 4-12 μm.

According to the surface straw acidification lubrication treatment method, a heat-resistant steel wire subjected to solid-solution heat treatment is activated by an etching activator, and an oxidation film generated on the surface of the wire in the solid-solution heat treatment process and components of the wire surface influencing straw film formation are removed, so that the surface activation degree of the wire is improved; then oxalic acid conversion agent is used for oxalic acid reaction, oxalic acid lubricating film with regular crystal shape, uniform size, 4-12 mu m range and coverage rate of 100% is formed on the surface of the wire rod, the oxalic acid lubricating film has good binding force and lubricating performance, the service life of the die in the wire rod drawing and cold heading forming process can be greatly prolonged, and the defects of cold heading cracking, galling and the like are reduced.

The beneficial effect that technical scheme that this application provided brought includes:

1. the treatment method provided by the application greatly reduces and shortens the temperature and time of the etching activation process, the temperature is reduced from the current 60 ℃ in the industry to 35-45 ℃, the time is shortened from 1 hour to 10-15 minutes, the long-time soaking of the material by the acid solution is avoided, and the performance damage to the heat-resistant steel wire rod is greatly reduced;

2. the treatment method provided by the application reduces the temperature of the oxalic acid treatment process from the current 90 ℃ in the industry to 65-70 ℃, and reduces the process control difficulty and energy consumption;

3. by utilizing the method for carrying out the etching activation and then the oxalic acid treatment, the oxalic acid lubricating film with regular crystallization can be formed, the lubricating property of the surface of the wire rod is improved, and the service life of the die and the cold heading forming property are prolonged.

Drawings

In order to more clearly illustrate the technical solutions in the embodiments of the present application, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present application, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.

Fig. 1 is a schematic flow chart of a surface oxalate lubrication treatment method for a heat-resistant steel wire rod according to an embodiment of the present application.

Detailed Description

In order to make the objects, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are some embodiments of the present application, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.

The embodiment of the application provides a surface straw acidification lubrication treatment method for a heat-resistant steel wire rod, which can solve the problems of high energy consumption and low lubrication performance in the related technology adopting the wire rod lubrication processes of common stainless steel SUS304, SUS316 and the like.

Fig. 1 is a schematic flow chart of a surface acidification and lubrication treatment method of a heat-resistant steel wire rod provided by the present application, and referring to fig. 1, the surface acidification and lubrication treatment method provided by the present application comprises the following steps:

step S101, soaking the heat-resistant steel wire subjected to solid melting treatment in an etching activator at 35-45 ℃ for activation for 10-15min, and cleaning the etching activator remained on the surface of the heat-resistant steel wire by using normal-temperature tap water after the activation is finished; wherein the etching activator comprises the following components in parts by mass: 20-25 parts of hydrochloric acid, 4-6 parts of sulfuric acid, 4-6 parts of nitric acid and 0.1-0.15 part of hexamethylenetetramine; the heat-resistant steel wire rod comprises the following chemical components in percentage by mass: c is less than or equal to 0.08, Si is less than or equal to 1.0, Mn is less than or equal to 2.0, P is less than or equal to 0.025, S is less than or equal to 0.01, Cr: 13.5-16.0, Ni: 24.0-27.0, Mo: 1.0-1.5, Ti: 1.75-2.35, Al is less than or equal to 0.35, V: 0.1-0.5, B: 0.001-0.01, and the balance of Fe;

step S102, immersing the cleaned heat-resistant steel wire rod into tap water at the temperature of 80-85 ℃ for primary drying;

step S103, soaking the heat-resistant steel wire rod dried for the first time in the step S102 in an oxalic acid conversion agent with the temperature of 65-70 ℃ for carrying out Chinese herbal medicine acidification treatment for 25-30min, and after the oxalic acid treatment is finished, soaking the heat-resistant steel wire rod in normal-temperature tap water for cleaning; wherein the oxalic acid conversion agent comprises the following components in parts by mass: 36-38 parts of oxalic acid, 8-9 parts of ferric sulfate, 3-4 parts of sodium bisulfite and 1-1.5 parts of sodium thiosulfate;

and step S104, immersing the heat-resistant steel wire rod cleaned in the step S103 into tap water at the temperature of 80-85 ℃ for secondary drying, standing at room temperature for cooling, and drying to obtain the heat-resistant steel wire rod with the oxalic acid lubrication film covered on the surface.

The method for surface acidification and lubrication treatment of the heat-resistant steel wire rod provided by the present application will be described in detail with reference to the following examples.

Example 1:

the embodiment 1 of the application provides a surface straw acidification and lubrication treatment method for a heat-resistant steel wire rod, which comprises the following steps:

step S101, soaking a heat-resistant steel wire rod which is subjected to solid melting heat treatment and has 14 wt% of chromium and 25 wt% of nickel in an etching activator at 45 ℃ for activation for 10min, and cleaning away the etching activator remaining on the surface of the heat-resistant steel wire rod by using normal-temperature tap water after the activation is finished;

step S102, immersing the cleaned heat-resistant steel wire rod in tap water at the temperature of 80 ℃ for 1 min;

step S103, soaking the heat-resistant steel wire rod dried for the first time in the step S102 in an oxalic acid conversion agent with the temperature of 65 ℃ for carrying out Chinese herbal medicine acidification treatment for 30min, and after the oxalic acid acidification treatment is finished, soaking the heat-resistant steel wire rod in tap water with the normal temperature for cleaning for 30S;

and step S104, immersing the heat-resistant steel wire rod cleaned in the step S103 in tap water at 82 ℃ for 1min, taking out the heat-resistant steel wire rod, standing in the air, and drying at the temperature of the heat-resistant steel wire rod to obtain the heat-resistant steel wire rod with the surface covered with the oxalated lubricating film.

In example 1, the components of the etching activator are shown in Table 1, and the components of the oxalic acid conversion agent are shown in Table 2.

Table 1: composition of etching activator used in example 1

Serial number	Component (A)	Mass concentration/(g/L)
			1	Hydrochloric acid	20
2	Sulfuric acid	4
			3	Nitric acid	4
4	Hexamethylenetetramine	0.1

Table 2: example 1 Components of the grass acidification conversion agent used

Serial number	Component (A)	Mass concentration/(g/L)
			1	Oxalic acid	36
2	Ferric sulfate	8
			3	Sodium bisulfite	3
4	Sodium thiosulfate	1

In example 1, 1g of the composition was one part by mass.

The oxalic acid-formed lubricating film formed on the surface of the heat-resistant steel wire rod in example 1 was examined for its properties, which are shown in Table 3.

Table 3: results of examining the Performance of oxalic acid-modified lubricating film of example 1

As can be seen from Table 3, the oxalic acid lubricating film obtained by the method has the performance meeting the lubricating requirements of drawing and cold heading forming of the heat-resistant steel wire.

Example 2:

the embodiment 2 of the application provides a surface straw acidification and lubrication treatment method for a heat-resistant steel wire rod, which comprises the following steps:

step S101, soaking a heat-resistant steel wire rod which is subjected to solid melting heat treatment and has a chromium content of 13.5 wt% and a nickel content of 24 wt% in an etching activator at 40 ℃ for activation for 13min, and cleaning away the etching activator residual on the surface of the heat-resistant steel wire rod by using normal-temperature tap water after the activation is finished;

step S102, immersing the cleaned heat-resistant steel wire rod in tap water at 83 ℃ for 1 min;

step S103, soaking the heat-resistant steel wire rod dried for the first time in the step S102 in an oxalic acid conversion agent with the temperature of 68 ℃ for carrying out Chinese herbal medicine acidification treatment for 27min, and after the oxalic acid treatment is finished, soaking the heat-resistant steel wire rod in normal-temperature tap water for cleaning for 30S;

and step S104, immersing the heat-resistant steel wire rod cleaned in the step S103 in tap water at 82 ℃ for 1min, taking out the heat-resistant steel wire rod, standing in the air, and drying at the temperature of the heat-resistant steel wire rod to obtain the heat-resistant steel wire rod with the surface covered with the oxalated lubricating film.

In example 2, the compositions of the etching activators are shown in Table 4, and the compositions of the oxalic acid conversion agents are shown in Table 5.

Table 4: components of etching activators used in example 2

Serial number	Component (A)	Mass concentration/(g/L)
			1	Hydrochloric acid	22
2	Sulfuric acid	5
			3	Nitric acid	5
4	Hexamethylenetetramine	0.13

Table 5: example 2 Components of the grass acidification conversion agent used

In example 2, 1g of the composition was one part by mass.

The oxalic acid lubricating film formed on the surface of the heat-resistant steel wire rod in example 2 was examined for properties, which are shown in Table 6.

Table 6: results of examining the Performance of oxalic acid-modified lubricating film of example 2

Detecting items	Require that	Results
			Crystal shape	Regular diamond	Regular diamond
Crystal size (. mu.m)	4-12	6-11
			Coverage (%)	100	100

As can be seen from Table 6, the oxalic acid lubricating film obtained by the method has the performance meeting the lubricating requirements of drawing and cold heading forming of the heat-resistant steel wire.

Example 3:

the embodiment 3 of the application provides a surface straw acidification and lubrication treatment method for a heat-resistant steel wire rod, which comprises the following steps:

step S101, soaking a heat-resistant steel wire rod which is subjected to solid melting heat treatment and has 14.5 wt% of chromium and 25.5 wt% of nickel in an etching activator at 35 ℃ for activation for 15min, and cleaning away the etching activator remained on the surface of the heat-resistant steel wire rod by using normal-temperature tap water after the activation is finished;

step S102, immersing the cleaned heat-resistant steel wire rod in tap water at 85 ℃ for 1 min;

step S103, soaking the heat-resistant steel wire rod dried for the first time in the step S102 in an oxalic acid conversion agent with the temperature of 65 ℃ for carrying out Chinese herbal medicine acidification treatment for 30min, and after the oxalic acid acidification treatment is finished, soaking the heat-resistant steel wire rod in tap water with the normal temperature for cleaning for 30S;

and step S104, immersing the heat-resistant steel wire rod cleaned in the step S103 in tap water at 82 ℃ for 1min, taking out the heat-resistant steel wire rod, standing in the air, and drying at the temperature of the heat-resistant steel wire rod to obtain the heat-resistant steel wire rod with the surface covered with the oxalated lubricating film.

In example 3, the compositions of the etching activators are shown in Table 7, and the compositions of the oxalic acid conversion agents are shown in Table 8.

Table 7: components of etching activators used in example 3

Serial number	Component (A)	Mass concentration/(g/L)
			1	Hydrochloric acid	25
2	Sulfuric acid	6
			3	Nitric acid	6
4	Hexamethylenetetramine	0.15

Table 8: example 3 composition of the grass acidification conversion agent used

Serial number	Component (A)	Mass concentration/(g/L)
			1	Oxalic acid	38
2	Ferric sulfate	9
			3	Sodium bisulfite	4
4	Sodium thiosulfate	1.5

In example 3, 1g of the composition was one part by mass.

The oxalic acid lubricating film formed on the surface of the heat-resistant steel wire rod in example 3 was examined for properties, which is shown in Table 9.

Table 9: results of examining the Performance of oxalic acid-modified lubricating film of example 3

Detecting items	Require that	Results
			Crystal shape	Regular diamond	Regular diamond
Crystal size (. mu.m)	4-12	6-10
			Coverage (%)	100	100

As can be seen from Table 9, the oxalic acid lubricating film obtained by the above method has properties meeting the lubricating requirements of drawing and cold heading forming of the heat-resistant steel wire.

Example 4:

the embodiment 4 of the application provides a surface straw acidification and lubrication treatment method for a heat-resistant steel wire rod, which comprises the following steps:

step S101, soaking a heat-resistant steel wire rod which is subjected to solid melting heat treatment and has a chromium content of 15 wt% and a nickel content of 24.5 wt% in an etching activator at 36 ℃ for activation for 12min, and after the activation is finished, cleaning away the etching activator residual on the surface of the heat-resistant steel wire rod by using normal-temperature tap water;

step S102, immersing the cleaned heat-resistant steel wire rod in tap water at the temperature of 81 ℃ for 1 min;

step S103, soaking the heat-resistant steel wire rod dried for the first time in the step S102 in an oxalic acid conversion agent with the temperature of 66 ℃ for carrying out Chinese herbal medicine acidification treatment for 28min, and after the oxalic acid treatment is finished, soaking the heat-resistant steel wire rod in tap water with the normal temperature for cleaning for 30S;

and step S104, immersing the heat-resistant steel wire rod cleaned in the step S103 in tap water at 83 ℃ for 1min, taking out the heat-resistant steel wire rod, standing in the air, and drying at the temperature of the heat-resistant steel wire rod to obtain the heat-resistant steel wire rod with the surface covered with the oxalated lubricating film.

In example 4, the respective compositions of the etching activators are shown in Table 10, and the respective compositions of the oxalic acid conversion agents are shown in Table 11.

Table 10: composition of etching activator used in example 4

Serial number	Component (A)	Mass concentration/(g/L)
			1	Hydrochloric acid	21
2	Sulfuric acid	4.5
			3	Nitric acid	5.5
4	Hexamethylenetetramine	0.12

Table 11: example 4 composition of grass acidification conversion agent used

Serial number	Component (A)	Mass concentration/(g/L)
			1	Oxalic acid	36.5
2	Ferric sulfate	8.4
			3	Sodium bisulfite	3.2
4	Sodium thiosulfate	1.4

In example 4, 1g of the composition was one part by mass.

The oxalic acid lubricating film formed on the surface of the heat-resistant steel wire rod in example 4 was examined for its properties, which is shown in Table 12.

Table 12: results of examining the Performance of oxalic acid-modified lubricating film of example 4

Detecting items	Require that	Results
			Crystal shape	Regular diamond	Regular diamond
Crystal size (. mu.m)	4-12	7-11
			Coverage (%)	100	100

As can be seen from Table 12, the oxalic acid lubricating film obtained by the above method has properties satisfying the lubricating requirements of the drawing and cold heading forming of the heat-resistant steel wire.

Example 5:

the embodiment 5 of the application provides a surface straw acidification and lubrication treatment method for a heat-resistant steel wire rod, which comprises the following steps:

step S101, soaking a heat-resistant steel wire rod which is subjected to solid melting heat treatment and has a chromium content of 15.5 wt% and a nickel content of 24.5 wt% in an etching activator at 37 ℃ for activation for 14min, and after the activation is finished, cleaning away the etching activator residual on the surface of the heat-resistant steel wire rod by using normal-temperature tap water;

step S102, immersing the cleaned heat-resistant steel wire rod in tap water at the temperature of 80 ℃ for 1 min;

step S103, soaking the heat-resistant steel wire rod dried for the first time in the step S102 in an oxalic acid conversion agent at 68 ℃ for carrying out Chinese herbal medicine acidification treatment for 29min, and after the oxalic acid treatment is finished, soaking the heat-resistant steel wire rod in normal-temperature tap water for cleaning for 30S;

and step S104, immersing the heat-resistant steel wire rod cleaned in the step S103 in tap water at 85 ℃ for 1min, taking out the heat-resistant steel wire rod, standing in the air, and drying at the temperature of the heat-resistant steel wire rod to obtain the heat-resistant steel wire rod with the surface covered with the oxalated lubricating film.

In example 5, the respective compositions of the etching activators are shown in Table 13, and the respective compositions of the oxalic acid conversion agents are shown in Table 14.

Table 13: components of etching activators used in example 5

Serial number	Component (A)	Mass concentration/(g/L)
			1	Hydrochloric acid	23.5
2	Sulfuric acid	4.8
			3	Nitric acid	4.2
4	Hexamethylenetetramine	0.13

Table 14: example 5 composition of grass acidification conversion agent used

Serial number	Component (A)	Mass concentration/(g/L)
			1	Oxalic acid	37
2	Ferric sulfate	8.7
			3	Sodium bisulfite	3.6
4	Sodium thiosulfate	1.2

In example 5, 1g of the composition was one part by mass.

The oxalic acid lubricating film formed on the surface of the heat-resistant steel wire rod in example 5 was examined for its properties, which is shown in Table 15.

Table 15: results of examining the Properties of oxalic acid-modified lubricating film of example 5

Detecting items	Require that	Results
			Crystal shape	Regular diamond	Regular diamond
Crystal size (. mu.m)	4-12	6-10
			Coverage (%)	100	100

As can be seen from Table 15, the oxalic acid lubricating film obtained by the above method has properties satisfying the lubricating requirements of the drawing and cold heading forming of the heat-resistant steel wire.

Example 6:

the embodiment 6 of the application provides a surface straw acidification and lubrication treatment method for a heat-resistant steel wire rod, which comprises the following steps:

step S101, soaking a heat-resistant steel wire rod which is subjected to solid melting heat treatment and has a chromium content of 13.5 wt% and a nickel content of 24 wt% in an etching activator at 35.5 ℃ for activation for 10min, and after the activation is finished, cleaning away the etching activator residual on the surface of the heat-resistant steel wire rod by using normal-temperature tap water;

step S102, immersing the cleaned heat-resistant steel wire rod in tap water at 84 ℃ for 1 min;

step S103, soaking the heat-resistant steel wire rod dried for the first time in the step S102 in an oxalic acid conversion agent at 66 ℃ for carrying out Chinese herbal medicine acidification treatment for 25min, and after the oxalic acid acidification treatment is finished, soaking the heat-resistant steel wire rod in normal-temperature tap water for cleaning for 30S;

and step S104, immersing the heat-resistant steel wire rod cleaned in the step S103 in tap water at 82 ℃ for 1min, taking out the heat-resistant steel wire rod, standing in the air, and drying at the temperature of the heat-resistant steel wire rod to obtain the heat-resistant steel wire rod with the surface covered with the oxalated lubricating film.

In example 6, the respective compositions of the etching activators are shown in Table 16, and the respective compositions of the oxalic acid conversion agents are shown in Table 17.

Table 16: composition of etching activator used in example 6

Table 17: example 6 composition of grass acidification conversion agent used

Serial number	Component (A)	Mass concentration/(g/L)
			1	Oxalic acid	37.5
2	Ferric sulfate	8.6
			3	Sodium bisulfite	3.1
4	Sodium thiosulfate	1.4

In example 6, 1g of the composition was one part by mass.

The oxalic acid lubricating film formed on the surface of the heat-resistant steel wire rod in example 6 was examined for its properties, which is shown in Table 18.

Table 18: results of examining the Properties of oxalic acid-modified lubricating film of example 6

Detecting items	Require that	Results
			Crystal shape	Regular diamond	Regular diamond
Crystal size (. mu.m)	4-12	6-11
			Coverage (%)	100	100

As can be seen from Table 18, the oxalic acid lubricating film obtained by the above method has properties satisfying the lubricating requirements of the drawing and cold heading forming of the heat-resistant steel wire rod.

Example 7:

the embodiment 7 of the application provides a surface straw acidification and lubrication treatment method for a heat-resistant steel wire rod, which comprises the following steps:

step S101, soaking a heat-resistant steel wire rod which is subjected to solid melting heat treatment and has 16 wt% of chromium and 24 wt% of nickel in an etching activator at 42 ℃ for activation for 10min, and cleaning away the etching activator remaining on the surface of the heat-resistant steel wire rod by using normal-temperature tap water after the activation is finished;

step S102, immersing the cleaned heat-resistant steel wire rod in tap water at the temperature of 80 ℃ for 1 min;

step S103, soaking the heat-resistant steel wire rod dried for the first time in the step S102 in an oxalic acid conversion agent with the temperature of 67 ℃ for carrying out Chinese herbal medicine acidification treatment for 28min, and after the oxalic acid treatment is finished, soaking the heat-resistant steel wire rod in tap water with the normal temperature for cleaning for 30S;

and step S104, immersing the heat-resistant steel wire rod cleaned in the step S103 in tap water at 84 ℃ for 1min, taking out the heat-resistant steel wire rod, standing in the air, and drying at the temperature of the heat-resistant steel wire rod to obtain the heat-resistant steel wire rod with the surface covered with the oxalated lubricating film.

In example 7, the respective compositions of the etching activators are shown in Table 19, and the respective compositions of the oxalic acid conversion agents are shown in Table 20.

Table 19: composition of etching activator used in example 7

Serial number	Component (A)	Mass concentration/(g/L)
			1	Hydrochloric acid	24.5
2	Sulfuric acid	4.6
			3	Nitric acid	4.2
4	Hexamethylenetetramine	0.12

Table 20: example 7 composition of grass acidification conversion agent used

Serial number	Component (A)	Mass concentration/(g/L)
			1	Oxalic acid	36.4
2	Ferric sulfate	8.6
			3	Sodium bisulfite	3.8
4	Sodium thiosulfate	1.4

In example 7, 1g of the composition was one part by mass.

The oxalic acid coated lubricating film formed on the surface of the heat-resistant steel wire rod in example 7 was examined for properties, which are shown in Table 21.

Table 21: results of examining the Properties of oxalic acid-modified lubricating film of example 7

Detecting items	Require that	Results
			Crystal shape	Regular diamond	Regular diamond
Crystal size (. mu.m)	4-12	5-11
			Coverage (%)	100	100

It can be seen from table 21 that the oxalic acid lubricating film obtained by the above method satisfies the lubricating requirements of the drawing and cold heading forming of the heat-resistant steel wire rod.

Example 8:

the embodiment 8 of the application provides a surface straw acidification and lubrication treatment method for a heat-resistant steel wire rod, which comprises the following steps:

step S101, soaking a heat-resistant steel wire rod which is subjected to solid melting heat treatment and has 16 wt% of chromium and 24 wt% of nickel in an etching activator at 43 ℃ for activation for 10min, and cleaning away the etching activator remained on the surface of the heat-resistant steel wire rod by using normal-temperature tap water after the activation is finished;

step S102, immersing the cleaned heat-resistant steel wire rod in tap water at 85 ℃ for 1 min;

step S103, soaking the heat-resistant steel wire rod dried for the first time in the step S102 in an oxalic acid conversion agent at 66 ℃ for carrying out Chinese herbal medicine acidification treatment for 25min, and after the oxalic acid acidification treatment is finished, soaking the heat-resistant steel wire rod in normal-temperature tap water for cleaning for 30S;

and step S104, immersing the heat-resistant steel wire rod cleaned in the step S103 in tap water at 82 ℃ for 1min, taking out the heat-resistant steel wire rod, standing in the air, and drying at the temperature of the heat-resistant steel wire rod to obtain the heat-resistant steel wire rod with the surface covered with the oxalated lubricating film.

In example 8, the respective compositions of the etching activators are shown in Table 22, and the respective compositions of the oxalic acid conversion agents are shown in Table 23.

Table 22: composition of etching activator used in example 8

Serial number	Component (A)	Mass concentration/(g/L)
			1	Hydrochloric acid	23
2	Sulfuric acid	5.5
			3	Nitric acid	4.5
4	Hexamethylenetetramine	0.14

Table 23: example 8 Components of the grass acidification conversion agent used

Serial number	Component (A)	Mass concentration/(g/L)
			1	Oxalic acid	37
2	Ferric sulfate	8.8
			3	Sodium bisulfite	3.2
4	Sodium thiosulfate	1.4

In example 8, 1g of the composition was one part by mass.

The oxalic acid lubricating film formed on the surface of the heat-resistant steel wire rod in example 8 was examined for its properties, which is shown in Table 24.

Table 24: results of examining the Properties of oxalic acid-modified lubricating film of example 8

Detecting items	Require that	Results
			Crystal shape	Regular diamond	Regular diamond
Crystal size (. mu.m)	4-12	6-10
			Coverage (%)	100	100

As can be seen from Table 24, the oxalic acid lubricating film obtained by the above method has properties satisfying the lubricating requirements of the drawing and cold heading forming of the heat-resistant steel wire.

Example 9:

the embodiment 9 of the application provides a surface straw acidification and lubrication treatment method for a heat-resistant steel wire rod, which comprises the following steps:

step S101, soaking a heat-resistant steel wire rod which is subjected to solid melting heat treatment and has 14.8 wt% of chromium and 26.5 wt% of nickel in an etching activator at 36 ℃ for activation for 10min, and cleaning away the etching activator residual on the surface of the heat-resistant steel wire rod by using normal-temperature tap water after the activation is finished;

step S102, immersing the cleaned heat-resistant steel wire rod in tap water at 82 ℃ for 1 min;

step S103, soaking the heat-resistant steel wire rod dried for the first time in the step S102 in an oxalic acid conversion agent with the temperature of 67 ℃ for carrying out Chinese herbal medicine acidification treatment for 30min, and after the oxalic acid acidification treatment is finished, soaking the heat-resistant steel wire rod in tap water with the normal temperature for cleaning for 30S;

and step S104, immersing the heat-resistant steel wire rod cleaned in the step S103 in tap water at 84 ℃ for 1min, taking out the heat-resistant steel wire rod, standing in the air, and drying at the temperature of the heat-resistant steel wire rod to obtain the heat-resistant steel wire rod with the surface covered with the oxalated lubricating film.

In example 9, the respective compositions of the etching activators are shown in Table 25, and the respective compositions of the oxalic acid conversion agents are shown in Table 26.

Table 25: composition of etching activator used in example 9

Serial number	Component (A)	Mass concentration/(g/L)
			1	Hydrochloric acid	24.5
2	Sulfuric acid	4.5
			3	Nitric acid	4.5
4	Hexamethylenetetramine	0.15

Table 26: example 9 Components of the grass acidification conversion agent used

Serial number	Component (A)	Mass concentration/(g/L)
			1	Oxalic acid	37.5
2	Ferric sulfate	8.5
			3	Sodium bisulfite	3.5
4	Sodium thiosulfate	1.2

In example 9, 1g of the composition was one part by mass.

The oxalic acid coated lubricating film formed on the surface of the heat-resistant steel wire rod in example 9 was examined for its properties, which are shown in Table 27.

Table 27: results of examining the Properties of oxalic acid-modified lubricating film of example 9

Detecting items	Require that	Results
			Crystal shape	Regular diamond	Regular diamond
Crystal size (. mu.m)	4-12	5-10
			Coverage (%)	100	100

As can be seen from Table 27, the oxalic acid lubricating film obtained by the above method has properties satisfying the lubricating requirements of the drawing and cold heading forming of the heat-resistant steel wire rod.

Example 10:

the embodiment 10 of the application provides a surface straw acidification and lubrication treatment method for a heat-resistant steel wire rod, which comprises the following steps:

step S101, soaking a heat-resistant steel wire rod which is subjected to solid melting heat treatment and has 15.5 wt% of chromium and 25 wt% of nickel in an etching activator at 43 ℃ for activation for 10min, and cleaning away the etching activator residual on the surface of the heat-resistant steel wire rod by using normal-temperature tap water after the activation is finished;

step S102, immersing the cleaned heat-resistant steel wire rod in tap water at 82 ℃ for 1 min;

step S103, soaking the heat-resistant steel wire rod dried for the first time in the step S102 in an oxalic acid conversion agent with the temperature of 68 ℃ for carrying out Chinese herbal medicine acidification treatment for 26min, and after the oxalic acid treatment is finished, soaking the heat-resistant steel wire rod in tap water with the normal temperature for cleaning for 30S;

and step S104, immersing the heat-resistant steel wire rod cleaned in the step S103 in tap water at 82 ℃ for 1min, taking out the heat-resistant steel wire rod, standing in the air, and drying at the temperature of the heat-resistant steel wire rod to obtain the heat-resistant steel wire rod with the surface covered with the oxalated lubricating film.

In example 10, the compositions of etching activators are shown in Table 28, and the compositions of oxalic acid conversion agents are shown in Table 29.

Table 28: composition of etching activator used in example 10

Serial number	Component (A)	Mass concentration/(g/L)
			1	Hydrochloric acid	20.5
2	Sulfuric acid	4.5
			3	Nitric acid	5.5
4	Hexamethylenetetramine	0.13

Table 29: example 10 Components of the grass acidification conversion agent used

Serial number	Component (A)	Mass concentration/(g/L)
			1	Oxalic acid	37
2	Ferric sulfate	8.1
			3	Sodium bisulfite	3.8
4	Sodium thiosulfate	1.4

In example 10, 1g of the composition was one part by mass.

The oxalic acid lubricating film formed on the surface of the heat-resistant steel wire rod in example 10 was examined for its properties, which is shown in Table 30.

Table 30: results of examining the Properties of oxalic acid-modified lubricating film of example 10

Detecting items	Require that	Results
			Crystal shape	Regular diamond	Regular diamond
Crystal size (. mu.m)	4-12	5-10
			Coverage (%)	100	100

As can be seen from Table 30, the oxalic acid lubricating film obtained by the above method has properties satisfying the lubricating requirements of the drawing and cold heading forming of the heat-resistant steel wire rod.

In the description herein, reference to the description of the terms "one embodiment/mode," "some embodiments/modes," "example," "specific example" or "some examples" or the like means that a particular feature, structure, material, or characteristic described in connection with the embodiment/mode or example is included in at least one embodiment/mode or example of the application. In this specification, the schematic representations of the terms used above are not necessarily intended to be the same embodiment/mode or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments/modes or examples. Furthermore, the various embodiments/aspects or examples and features of the various embodiments/aspects or examples described in this specification can be combined and combined by one skilled in the art without conflicting therewith.

It is noted that, in the present application, relational terms such as "first" and "second", and the like, are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element. In this application, "plurality" means at least two, e.g., two, three, etc., unless specifically stated otherwise.

The above description is merely exemplary of the present application and is presented to enable those skilled in the art to understand and practice the present application. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the application. Thus, the present application is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.