阅读说明：本技术 钛合金及纯钛容器内壁表面处理工艺 (Titanium alloy and pure titanium container inner wall surface treatment process ) 是由 董兴玉 刘民 于 2021-08-26 设计创作，主要内容包括：本发明涉及钛合金及纯钛容器内壁表面处理工艺,包括如下步骤：S1、对产品内壁进行精细抛光；S2、对钛合金及纯钛容器专用表面处理剂进行加热；S3、抛光后的容器浸泡在温度为60℃的除油剂中,浸泡时间不少于30min；S4、将容器取出,并用流动的洁净水冲洗容器内表面不少于2min；S5、再用无油、无水的洁净压缩空气对容器内部进行吹扫,吹扫时间不少于2min；S6、再用无尘布蘸取高纯度酒精擦拭容器内表面；S7、把加热到70～90℃的表面处理剂通过自动化设备灌入钛合金或纯钛容器中,并静置5-10min；S8、倒出表面处理剂到回收桶中；S9、用洁净自来水冲洗容器内壁3次,每次冲洗时间不少于5min；S10、容器放置在洁净室内,自然晾干,使表面成膜更稳定。(The invention relates to a surface treatment process for the inner wall of a titanium alloy and pure titanium container, which comprises the following steps: s1, finely polishing the inner wall of the product; s2, heating the special surface treating agent for the titanium alloy and the pure titanium container; s3, soaking the polished container in a degreasing agent at the temperature of 60 ℃ for not less than 30 min; s4, taking out the container, and washing the inner surface of the container for not less than 2min by using flowing clean water; s5, purging the interior of the container by using oil-free and water-free clean compressed air for not less than 2 min; s6, dipping the inner surface of the container with high-purity alcohol by using a dust-free cloth to wipe the inner surface of the container; s7, pouring the surface treating agent heated to 70-90 ℃ into a titanium alloy or pure titanium container through automatic equipment, and standing for 5-10 min; s8, pouring the surface treating agent into a recycling bin; s9, washing the inner wall of the container for 3 times by using clean tap water, wherein the washing time is not less than 5min each time; s10, placing the container in a clean room, and naturally airing to enable the surface film to be more stable.)

1. The surface treatment process for the inner wall of the titanium alloy and pure titanium container is characterized by comprising the following steps of:

s1, finely polishing the inner wall of the product;

s2, heating the special surface treating agent for the titanium alloy and the pure titanium container;

s3, soaking the polished container in a degreasing agent at the temperature of 60 ℃ for not less than 30 min;

s4, taking out the container, and washing the inner surface of the container for not less than 2min by using flowing clean water;

s5, purging the interior of the container by using oil-free and water-free clean compressed air for not less than 2 min;

s6, dipping the inner surface of the container with high-purity alcohol by using a dust-free cloth to wipe the inner surface of the container;

s7, pouring the surface treating agent heated to 70-90 ℃ into a titanium alloy or pure titanium container through automatic equipment, and standing for 5-10 min;

s8, pouring the surface treating agent into a recycling bin;

s9, washing the inner wall of the container for 3 times by using clean tap water, wherein the washing time is not less than 5min each time;

s10, placing the container in a clean room, and naturally airing to enable the surface film to be more stable.

2. The process for treating the inner wall surface of a titanium alloy and pure titanium container according to claim 1, wherein: the surface roughness is not more than 0.1 μm after polishing in the step S1.

3. The process for treating the inner wall surface of a titanium alloy and pure titanium container according to claim 1, wherein: the heating temperature in the step S2 is 70-90 ℃.

4. The process for treating the inner wall surface of a titanium alloy and pure titanium container according to claim 1, wherein: and the cleanliness of the clean room in the step S10 is not lower than 1000 grade.

5. The process for treating the inner wall surface of a titanium alloy and pure titanium container according to claim 1, wherein: the surface treatment agent comprises the following components in percentage by volume: 19-29 parts of nitric acid; 1-5 parts of sulfonic acid; 1-3 parts of diphosphonic acid; 1-5 parts of monobutyl ether; 1 part of zeolite; 5 parts of adsorbent; 62 parts of water.

6. The process for treating the inner wall surface of a titanium alloy and pure titanium container according to claim 1, wherein: the container is a titanium alloy or pure titanium container.

Technical Field

The invention relates to the technical field of container inner wall surface treatment processes, in particular to a titanium alloy and pure titanium container inner wall surface treatment process for the liquid crystal industry.

Background

The inner wall surfaces of titanium alloy and pure titanium containers applied to the liquid crystal industry at present are dirty, the cleanliness is insufficient, the titanium alloy and pure titanium containers are not used for containing chemical materials with higher purity, the chemical materials corrode the surfaces of the containers, the container base materials can possibly react with the filled chemical materials, and the like, so that the quality of the liquid crystal materials contained in the containers cannot be guaranteed. In order to meet the requirements of customers and ensure the quality of stored chemicals, the inner wall of titanium alloy and pure titanium containers needs to be subjected to surface treatment to improve the cleanliness of the inner wall.

Disclosure of Invention

In order to solve the technical problems, the invention aims to solve the problems of insufficient cleanliness, corrosion resistance and the like of the inner wall surfaces of titanium alloys and pure titanium containers, and provides an inner wall surface treatment process method with reasonable design and simple process. The invention can improve the internal cleanliness of the packaging container, reduce the influence on the chemical materials contained in the packaging container, and increase the corrosion resistance of the container wall, thereby ensuring the quality of the chemicals contained in the container applied to the liquid crystal industry.

The technical scheme of the invention is as follows:

the surface treatment process for the inner wall of the titanium alloy and pure titanium container is characterized by comprising the following steps of:

s1, finely polishing the inner wall of the product;

s2, heating the special surface treating agent for the titanium alloy and the pure titanium container;

s3, soaking the polished container in a degreasing agent at the temperature of 60 ℃ for not less than 30 min;

s4, taking out the container, and washing the inner surface of the container for not less than 2min by using flowing clean water;

s5, purging the interior of the container by using oil-free and water-free clean compressed air for not less than 2 min;

s6, dipping the inner surface of the container with high-purity alcohol by using a dust-free cloth to wipe the inner surface of the container;

s7, pouring the surface treating agent heated to 70-90 ℃ into a titanium alloy or pure titanium container through automatic equipment, and standing for 5-10 min;

s8, pouring the surface treating agent into a recycling bin;

s9, washing the inner wall of the container for 3 times by using clean tap water, wherein the washing time is not less than 5min each time;

s10, placing the container in a clean room, and naturally airing to enable the surface film to be more stable.

Further, the surface roughness of the polished film in the step S1 is not more than 0.1 μm.

Further, the heating temperature in the step S2 is 70-90 ℃.

Further, the cleanliness of the clean room in the step S10 is not lower than 1000.

Furthermore, the container is a titanium alloy or pure titanium container.

Further, the surface treatment agent comprises the following components in percentage by volume: 19-29 parts of nitric acid; 1-5 parts of sulfonic acid; 1-3 parts of diphosphonic acid; 1-5 parts of monobutyl ether; 1 part of zeolite; 5 parts of adsorbent; 62 parts of water.

By the scheme, the invention at least has the following advantages:

the surface treatment process of the present invention is a technological process of forming one layer of protecting film with mechanical and chemical performance different from that of the inner wall base material on the inner wall surface of titanium alloy or pure titanium container through a series of chemical reactions. The method can change the material performance of the inner wall of the original titanium alloy or pure titanium container, form an oxidation film on the surface of the original material, increase the corrosion resistance of the container wall and improve the cleanliness of the interior of the container.

The foregoing is a summary of the present invention, and in order to provide a clear understanding of the technical means of the present invention and to be implemented in accordance with the present specification, the following is a detailed description of the preferred embodiments of the present invention.

Detailed Description

The following examples are given to further illustrate the embodiments of the present invention. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.

Example 1:

finely polishing the inner wall of the product to ensure that the surface has no defects of scratches, sand holes, coarse grains and the like after visual inspection, the surface brightness and the glossiness are consistent, and the surface roughness is not more than 0.1 mu m after polishing; heating the special surface treating agent for the titanium alloy and the pure titanium container at the temperature of 70 ℃; soaking the polished container in an oil removing agent at 60 deg.C for at least 30min to remove residual oil; taking out the container, and washing the inner surface of the container with flowing clean water for at least 2min to prevent dirt residue; then, oil-free and water-free clean compressed air is used for purging the interior of the container, the purging time is not less than 2min, and the evaporation of residual water in the interior of the container is accelerated; then, dipping high-purity alcohol by using a dust-free cloth to wipe the inner surface of the container, taking away residual water, paying attention to gentle action in the wiping process, and prohibiting scratching and touching the inner surface; pouring the surface treating agent heated to 70 ℃ into a titanium alloy or pure titanium container through automatic equipment; standing for 5 min; pouring the surface treating agent into a recycling bin; washing the inner wall of the container with clean tap water for 3 times, wherein the washing time is not less than 5min each time, so as to avoid the residue of the surface treatment agent; the container is placed in a clean room with the cleanliness of not less than 1000 grade and is naturally dried, so that the surface film forming is more stable.

The formulation of the treating agent in example 1 is that 100L of an acid-resistant and corrosion-resistant open container is prepared; calculating the volume required by each raw material according to the volume ratio (19L of nitric acid, 5L of sulfonic acid, 3L of diphosphonic acid, 5L of monobutyl ether, 1L of zeolite, 62L of water and 5L of other adsorbents); filling the calculated corresponding volume of water 62L into the container; slowly adding 19L of nitric acid into the required water, and quickly stirring for heat dissipation; when the temperature of the nitric acid solution is recovered to the normal temperature, adding 3L of diphosphoric acid into the solution, and uniformly stirring; and adding 5L of sulfonic acid, 5L of monobutyl ether, 1L of other surfactant, 5L of adsorbent and the like into the solution, and uniformly stirring to obtain the surface treatment solution for the inner wall of the packaging container.

Example 2:

finely polishing the inner wall of the product to ensure that the surface has no defects of scratches, sand holes, coarse grains and the like after visual inspection, the surface brightness and the glossiness are consistent, and the surface roughness is not more than 0.1 mu m after polishing; heating the surface treating agent special for titanium alloy and pure titanium containers at 80 ℃; soaking the polished container in an oil removing agent at 60 deg.C for at least 30min to remove residual oil; taking out the container, and washing the inner surface of the container with flowing clean water for at least 2min to prevent dirt residue; then, oil-free and water-free clean compressed air is used for purging the interior of the container, the purging time is not less than 2min, and the evaporation of residual water in the interior of the container is accelerated; then, dipping high-purity alcohol by using a dust-free cloth to wipe the inner surface of the container, taking away residual water, paying attention to gentle action in the wiping process, and prohibiting scratching and touching the inner surface; pouring the surface treating agent heated to 80 ℃ into a titanium alloy or pure titanium container through automatic equipment; standing for 8 min; pouring the surface treating agent into a recycling bin; washing the inner wall of the container with clean tap water for 3 times, wherein the washing time is not less than 5min each time, so as to avoid the residue of the surface treatment agent; the container is placed in a clean room with the cleanliness of not less than 1000 grade and is naturally dried, so that the surface film forming is more stable.

The formulation of the treating agent in example 2 is that 100L of an acid-resistant and corrosion-resistant open container is prepared; calculating the volume required by each raw material according to the volume ratio (29L of nitric acid, 1L of sulfonic acid, 1L of diphosphonic acid, 1L of monobutyl ether, 1L of zeolite, 62L of water, 5L of other adsorbents); filling the calculated corresponding volume of water 62L into the container; slowly adding 29L of nitric acid into the required water, and quickly stirring for heat dissipation; when the temperature of the nitric acid solution is recovered to normal temperature, adding 1L of diphosphonic acid into the solution, and uniformly stirring; and adding 1L of sulfonic acid, 1L of monobutyl ether, 1L of other surfactants, 5L of adsorbent and the like into the solution, and uniformly stirring to obtain the surface treatment solution for the inner wall of the packaging container.

Example 3:

finely polishing the inner wall of the product to ensure that the surface has no defects of scratches, sand holes, coarse grains and the like after visual inspection, the surface brightness and the glossiness are consistent, and the surface roughness is not more than 0.1 mu m after polishing; heating the special surface treating agent for the titanium alloy and the pure titanium container at 90 ℃; soaking the polished container in an oil removing agent at 60 deg.C for at least 30min to remove residual oil; taking out the container, and washing the inner surface of the container with flowing clean water for at least 2min to prevent dirt residue; then, oil-free and water-free clean compressed air is used for purging the interior of the container, the purging time is not less than 2min, and the evaporation of residual water in the interior of the container is accelerated; then, dipping high-purity alcohol by using a dust-free cloth to wipe the inner surface of the container, taking away residual water, paying attention to gentle action in the wiping process, and prohibiting scratching and touching the inner surface; pouring the surface treating agent heated to 90 ℃ into a titanium alloy or pure titanium container through automatic equipment; standing for 10 min; pouring the surface treating agent into a recycling bin; washing the inner wall of the container with clean tap water for 3 times, wherein the washing time is not less than 5min each time, so as to avoid the residue of the surface treatment agent; the container is placed in a clean room with the cleanliness of not less than 1000 grade and is naturally dried, so that the surface film forming is more stable.

The formulation of the treating agent in example 3 is that 100L of an acid-resistant and corrosion-resistant open container is prepared; calculating the volume required by each raw material according to the volume ratio relationship (24L of nitric acid, 3L of sulfonic acid, 2L of diphosphonic acid, 3L of monobutyl ether, 1L of zeolite, 62L of water, 5L of other adsorbents); filling the calculated corresponding volume of water 62L into the container; slowly adding 24L of nitric acid into the required water, and quickly stirring for heat dissipation; when the temperature of the nitric acid solution is recovered to normal temperature, adding 2L of diphosphonic acid into the solution, and uniformly stirring; and adding 3L of sulfonic acid, 3L of monobutyl ether, 1L of other surfactant, 5L of adsorbent and the like into the solution, and uniformly stirring to obtain the surface treatment solution for the inner wall of the packaging container.

Example analysis:

1. corrosion resistance of inner wall of container

The results of the inner wall neutral salt spray test (120H) of the containers completed in the above examples and the packaging containers without surface treatment are shown in table 1:

TABLE 1

As can be seen from the above table, the inner wall of the packaging container surface-treated using the present invention is superior in corrosion resistance to the non-surface-treated inner wall, and the present invention is shown by comparison to increase the corrosion resistance of the inner wall of the container.

2. Cleanliness of container interior

The inner wall of the container after surface treatment is filled with the surface gaps of the inner wall, the separation of particles among the inner wall gaps is reduced, the content of the particles per cubic meter (more than or equal to 0.1 micron) in the container after vacuum pumping is 0, the cleanliness in the container is greatly improved, and then chemical materials with higher purity (99.999999%) can be contained, and the higher requirements of customers are met.

The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, it should be noted that, for those skilled in the art, many modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.