Shulou(Shulou.com)11/24 Report--

Japan has been leading the world in semiconductors with equipment and materials, and a ban in 2019 grabbed South Korean semiconductors by the throat, involving materials including high-purity hydrogen fluoride, fluoropolyimide and photoresist until a few months ago. the injured parties shook hands and made peace.

Why is high purity hydrogen fluoride juxtaposed with photoresist? It is a wet electronic chemical (Wet Chemicals), similar to electronic gas, as the "blood" of semiconductor products, without which chips cannot be produced.

This article is the 26th article in the series of "domestic substitution" planned by "Fruit Shell hard Science and Technology", focusing on wet electronic chemicals. In this article, you will learn which wet electronic chemicals will be used in semiconductor production, what are the special requirements, the current situation at home and abroad and the way forward for domestic development.

Fu Bin, author

Li Tuo (Editor)

1, the nobility in the liquid, the whole body is a barrier industry, wet electronic chemicals have many names, internationally it is called process chemicals (Process Chemicals), domestic is called "electronic grade reagents", "ultra-clean high-purity chemical reagents" and so on.

14% of wafer manufacturing materials are spent on wet electronic chemicals [1], which is used for chip cleaning, corrosion and wafer cleaning, which determines the final yield, electrical performance and reliability. [2]

For example, after the end of the lithography process, the etching process needs to use a specific etching solution to react with the film; after etching, the unexposed part of the photoresist needs to be dissolved by the stripping solution; during the whole production process, it is inevitable to be contaminated with dust, particles, metals or ionic conductive pollutants, and the cleaning solution can remove these impurities; in the metallization process, copper plating solution is an indispensable chemical in the copper interconnection process.

In addition to integrated circuits, flat panel displays and solar cells are also inseparable from wet electronic chemicals, because of their strong functionality, high added value, and the ability to transmit to the performance of terminal products. Therefore, the industry generally believes that wet electronic chemicals is an important lever to pry the industry.

Materials are an important support of the semiconductor industry [3] strictly speaking, as long as the liquids, pastes and stickies in the semiconductor production process are all wet electronic chemicals, but the wet electronic chemicals mentioned by the industry generally refer to ultra-high purity reagents.

There is no room for any grain of sand in chip manufacturing. Metal ions and non-metal ion impurities such as boron, silicon, arsenic, phosphorus, sulfur, chlorine and organic carbon in wet electronic chemicals will also directly affect the 3D structure of the chip. [4]

The harm of impurities to integrated circuits [5] the wet chemicals used in the semiconductor industry are known as aristocrats in the chemical industry, and the purity requirements are the highest.

In terms of purity, SEMI international standards are implemented all over the world, which are divided into five grades according to metal impurities, controlled particle size, number of particles and IC linewidth. G5 is the highest grade, and different grades are suitable for different applications. Among them, solar photovoltaic generally only needs G1 level, display panel and LED are generally G2~G3 level, semiconductors correspond to G4~G5, and the technical barrier is the highest.

SEMI International Standard Grade for Wet Electronic Chemicals [6]

There are many kinds of wet electronic chemicals used in integrated circuits, which can be divided into two categories: general wet chemicals and functional wet chemicals according to their composition and process.

General-purpose wet electronic chemicals are liquid chemicals widely used in the manufacturing process, which are generally single-component and single-function chemicals, such as hydrofluoric acid, sulfuric acid, nitric acid, phosphoric acid, hydrochloric acid, hydrogen peroxide, sodium hydroxide, potassium hydroxide, etc.

Functional wet electronic chemicals are compound chemicals that meet the needs of special manufacturing processes, such as developer, stripping solution, etching solution, diluent, cleaning solution, etc., involving photolithography, etching, ion implantation, CMP and other processes. [6]

Classification and specific products of wet electronic chemicals, tabulation, fruit shell hard science and technology

Reference materials: Glinda prospectus [6], Jingrui Electric material 2022 Annual report [7]

Specifically, the consumption of sulfuric acid, hydrofluoric acid, nitric acid, phosphoric acid, hydrochloric acid, hydrogen peroxide, ammonia and isopropanol in general chemicals is particularly large, while the consumption of diluent, developer, etching solution, stripping solution, buffer oxide etching agent (BOE), cleaning solution and electroplating solution in functional chemicals increases with the complexity of the process.

For chips, the more advanced the process, the greater the use of wet electronic chemicals. SEMI statistics show that the total process steps from 28nm to 5nm will increase from 400 to more than 1200, further driving the increase in the use of wet electronic chemicals. [3]

The use of some commonly used electronic grade chemicals, tabulation (fruit shell hard technology)

Reference materials: "Micro / Nano Electronics and Intelligent Manufacturing" [8], Shanghai Chemical Industry [9], China International Capital Corporation [10]

Of course, not only should the liquid itself be pure, but it should also be clean enough in the process of packaging, transportation and use. it can be said that there are technical barriers in every link of wet electronic chemicals:

Raw material impurity removal: raw material is the key to the preparation of high purity wet electronic chemicals. in terms of efficient impurity removal, the selection of impurity removal agents, the improvement of process parameters and the optimization of impurity removal system all need to be invested. [11]

Purification: the focus of purification of wet electronic chemicals is not on content, but on the removal of harmful metal ion content and particle content. Purification methods mainly include distillation and precision fractionation, ion exchange, molecular sieve separation, gas absorption and ultra-clean filtration. Several purification technologies have their own advantages; [9]

Mixing: proportioning and formula are the key, just like blending seasoning, not only experienced, but also in line with taste preferences. In addition, the blending process temperature, pressure, flow rate, ratio, exhaust and other indicators are closely related to the blending results.

Application of by-products: there are a large number of by-products in the production process of most wet electronic chemicals, such as barium fluorosilicate, which is a by-product in the process of removing impurities from electronic grade hydrofluoric acid, which can be sold directly after repeated washing and drying. therefore, the cascade utilization and development of by-products is the focus of production enterprises.

Detection: in the process of chip manufacturing, the pollution of wet electronic chemicals determines the lifeline of the enterprise. as the chip steps into the nanometer level, the requirements for metal and non-metallic impurities have reached the order of 10-12. In the past, the traditional GF-AAS and ICP-OES trace element detection methods have been eliminated, and now the commonly used analysis and testing methods are ICP-MS and ICP-MS / MS ion chromatography. At present, foreign analysis systems include ESI of the United States, IAS of Japan, Jin Zhaoyi of Taiwan, and domestic analysis systems include Hangzhou Science and Technology of China, etc.

Packaging and transportation: most of the wet electronic chemicals are flammable, explosive and highly corrosive dangerous goods, which can neither be leaked nor polluted in the process of transportation. at present, the most widely used packaging materials are high density polyethylene (HDPE), tetrafluoroethylene and fluoroalkyl vinyl ether copolymer (PFA), polytetrafluoroethylene (PTFE). The packaging requirements for different chemicals are also different.

Recycling: in chip production, the discharge of waste liquid is very astonishing, most of which are biotoxic and pollute the environment. Recycling is not only of environmental significance, but also can reduce the consumption of chemicals in enterprises. So far, wet electronic chemicals are mostly used for cleaning and drying, the content of impurities after use is not much, and most of the types of impurities are known, directional removal of impurities can be reused to reduce the cost of enterprises. [8]

2. From domestic substitute to well-off society

Customers of wet electronic chemicals for integrated circuits are more specialized, but they also have a certain market scale. According to the data of China Electronic Materials Industry Association and TECHCET, the global market scale of wet chemicals for integrated circuits will grow from US $5.69 billion to US $6.381 billion from 2022 to 2025. Affected by the reduced demand for downstream chips, the global market will reach US $5.1 billion in 2023, a slight decline over the same period last year, among which the overall market size of China will grow to US $1.027 billion in 2025. [3] [12]

In terms of key category chemistry, sulfuric acid, hydrogen peroxide, Cu PERR (post-etching cleaning agent) and CMP polishing solution are the top four wet electronic chemicals used in the world in 2023, accounting for 23%, 20%, 14% and 14%, respectively, followed by ammonia, phosphoric acid, AI PERR (post-etching cleaning agent), hydrofluoric acid, isopropanol, hydrochloric acid and nitric acid.

Wet electronic chemicals market segment [12] generation products, first generation materials, wet electronic chemicals technology threshold is high, large investment, rapid upgrading, coupled with China started decades later than foreign countries, it is not easy to compete in the market.

At present, large manufacturers in Europe, the United States, Japan and South Korea account for more than 70% of the global market for wet electronic chemicals, and the pattern is relatively stable. Europe and the US account for about 32 per cent of the global market, Japan 29 per cent and Chinese mainland only 12 per cent, according to the data. [13]

In terms of products, domestic products are mainly concentrated in low-end products such as solar cells, with low technical threshold and fierce competition; middle-end flat panel display and semiconductor products compete with each other; and high-end products are dominated by Germany, the United States and Japan. [14]

2021 global wet chemical market pattern (by sales) [13] Europe and the United States established chemical companies generally product grade G4 or above, and semiconductor chip manufacturing industry development almost at the same pace, representative companies including Germany BASF (Basf), Germany Merck (E.Merck), the United States Ashland (Ashland), the United States Arch Chemicals, the United States Honeywell (Honeywell), the United States Mallinckradt Baker, the United States Avantor Performance Materials, the United States ATMI and so on. [15]

Although the development of Japanese industry is later than that of Europe and America, it is developing fast. at present, the level of technology is basically the same as that of European and American enterprises, including Kanto Chemical, Mitsubishi Chemical, Kyoto Chemical, Japanese synthetic Rubber, Sumitomo Chemical, Hoguang Pure Pharmaceutical Industry (Wako), Ubu (UBE), Stella-Chemifa and so on. [5]

Wet electronic chemicals in South Korea and Taiwan are also developing at a high speed, and their production technology and process level can compete with Europe, the United States and Japan in high-end fields. representative enterprises include Korea Dongyou Fine Chemical, Korea Dongjin Shimeken, Taiwan Dongying Chemical, China Taiwan Lianshi Electronic Chemistry, Xinlin Technology and so on.

International representative enterprises of wet electronic chemicals [6] Wet electronic chemicals in China have made some breakthroughs and initially formed an industrial scale in general chemicals, but in terms of ultra-high purity reagents, both quality and quantity are difficult to meet the needs of the electronic industry. Chinese mainland enterprises accounted for only 9% of the Chinese market supply of ultra-clean and high-purity chemicals in 2019. [16]

Data show that the overall demand for wet electronic chemicals in China increased to 2.6169 million tons in 2022, compared with 2.1352 million tons last year, and is expected to reach 3.0703 million tons in 2023. Among them, the demand of integrated circuit, display panel and photovoltaic industry is 965900 tons, 1.166 million tons and 938400 tons respectively. It is estimated that by 2025, the total domestic demand will increase to 3.7 million tons, of which the demand for integrated circuits, display panels and photovoltaic industries will be 1.0694 million tons, 1.495 million tons and 1.1312 million tons respectively. [7]

The demand is not equal to the market, the more high-end the product is, the higher the value is. In 2021, the market size of China's wet electronic chemicals is 13.78 billion yuan, of which the market size of integrated circuits, display panels and photovoltaic industries is 5.2 billion yuan, 6.2 billion yuan and 1.7 billion yuan respectively, accounting for 40%, 47% and 13% respectively. The domestic market is expected to grow from 16.39 billion yuan to 30.17 billion yuan from 2022 to 2028. [7]

The scale of demand for wet electronic chemicals in China's three major application markets [13] at present, the overall localization rate of wet electronic chemicals in China is about 35%, and that of wet electronic chemicals for integrated circuits is about 23%. Among them, the domestic yield of hydrofluoric acid for high-end semiconductors is about 30%, nitric acid is about 50%, hydrochloric acid is about 20%, sulfuric acid is about 10%, ammonia is about 40%, hydrogen peroxide is about 70% [11]. The application of products such as NMP and tetramethyl ammonium hydroxide in high-end fields is still blank. [17]

Having said that, China has made rapid progress. At present, it has achieved a full range of domestic substitutes for integrated circuits, flat panel displays and solar cells, in other words, there are at least products available in every field.

So far, there are more than 40 domestic enterprises engaged in the research and production of wet chemicals, which are divided into three categories: professional suppliers of wet electronic chemicals, electronic materials platform enterprises and large chemical enterprises [18]. Including Jiangyin Jiangyin Chemical Micro, Jiangyin Runma Electronics, Jiangsu Essen, Zhejiang Kaisheng Fluorine, Jingrui Electronics, Hangzhou Glinda, Hubei Xingfu Electronics, Mid-Core Science and Technology, Duofuo, Anji Micro, Shanghai Xinyang, Cangzhou Xinlian, Wuxi Sankai, Zhenjiang Runjing, etc., customers have no lack of TSMC, SMIC, Changdian Technology, Huarun Micro, Silan Micro and other advanced foundry, packaging factory, IDM company.

Specifically, electronic grade nitric acid, hydrofluoric acid and phosphoric acid have made great breakthroughs and have entered the international supply chain. Electronic grade sulfuric acid, hydrochloric acid, ammonia and hydrogen peroxide have been partially applied in batch in China [16]. For example, Jianghua micro electronic grade hydrofluoric acid / sulfuric acid / nitric acid, Hubei Xingfu electronic grade phosphoric acid / sulfuric acid / silicon etching solution / aluminum etching solution, Jingrui electric material and Suzhou Jingrui electronic grade hydrogen peroxide, Shanghai Xinyang electronic grade sulfuric acid / copper plating solution / copper post-etching cleaning solution, Anji micro copper polishing cleaning solution has been applied in batch in 8-inch integrated circuit production line. Wet electronic chemicals for wafer manufacturing over 12-inch 28nm technology nodes have been used in a small number of applications, most of them are in the system certification stage, and the technologies below 28nm are in the stage of laboratory research and pilot development. [19]

Incomplete statistics of wet electronic chemical manufacturers in China, tabulation (fruit shell hard science and technology)

Reference materials: Glinda prospectus [6], Ping an Securities [20]

In recent years, driven by the domestic substitute demand and the semiconductor trade war between Japan and South Korea, the market output of wet electronic chemicals in China has been increasing. From 2016 to 2022, production increased from 240000 tons to 800000 tons, with a year-on-year increase of 23.1% in 2022. Not only that, there will be a lot of new production capacity in China by 2025.

New capacity planning for wet electronic chemicals in enterprises from 2022 to 2025 [20] domestic substitution is only the first step at this stage, and we still have to face the problem when we move towards a well-off society: domestic enterprises have relatively single products and lack leading enterprises with high market share of many varieties; although some enterprises have made breakthroughs in multi-variety products, their leading products are still limited, especially in the advanced process. [13]

3. If you want to make money, it is not easy to make wet electronic chemicals around the industry chain, and it is even more difficult to make money from it.

According to the financial reports of domestic companies, the overall gross profit margin fluctuates at 20% to 50%, functional wet electronic chemicals at 30% to 60%, high-end products to 70%, and general wet electronic chemicals at 5% to 30%.

On the contrary, the global chemical manufacturers are expanding cautiously because of the high threshold of wet electronic chemicals technology, large R & D investment and long R & D cycle. The SIA report mentioned that there is a shortage of wet electronic chemicals in some chip factories in the United States almost every year. [21]

Most of the international leading enterprises are all-round experts in the field of materials. with more types, they can avoid periodic risks, form industrial chains and networks, and maximize the value of raw materials, intermediates, by-products and so on. This point can be seen in the patent.

Using semiconductors and wet electronic chemicals as keywords to search on the wisdom bud, there are 19421 patents in 170 countries, with a total patent value of US $1.313 billion. Among them, the United States ranks first in the number of applications, accounting for 35.84% of the global patents related to wet electronic chemicals, followed by Japan, China, South Korea and Europe, accounting for 19.75%, 19.36%, 10.59% and 7.6% of the global total, respectively. It should be emphasized that there is a lack of patents going out to sea in China, while the relevant patents in the United States and Japan are in good condition.

Most of the enterprises in the forefront of patents are super-large integrated chemical enterprises, including BASF in Germany, LG Chemical in South Korea, Fuji in Japan, Sumitomo Chemical in Japan, DuPont in the United States and so on. On the other hand, the number of patents of domestic enterprises such as Hubei Xingfu, Jiangyin Runma and Jiangyin Jianghua Wei are also catching up with and surpassing foreign enterprises.

According to the analysis of typical applicants for wet electronic chemicals, the three major materials of semiconductors, such as fluorine-containing electronic gases, wet electronic chemicals and photoresist, have similar industrial logic.

According to the layout of six global leading companies, namely, BASF, Linde, Merck, Sumitomo Chemical of Japan, Mitsubishi Chemical of Japan and DuPont of the United States, five have dabbled in the field of wet electronic chemicals and photoresist, and cover stripping, cleaning, development, polishing and other related patents.

Comparison of technology layout of patent-based electronic chemicals segment in leading enterprises [22] the leader is not achieved overnight. Wet electronic chemicals were first used in the 1960s, and the international has been reshuffled and integrated for many times. At present, the global wet electronic chemicals are in a stable growth period, and it is expected to enter the mature stage after 5-20 years.

Technology maturity based on patent data computing [22]

The development of the business model of the leading national chemical reagent industry is mainly divided into three stages: the first stage, to achieve self-production and marketing through independent management; the second stage, to develop in the direction of supporting equipment, reagents and services to achieve full product line supply; and the third stage, cultivate R & D and marketing networks, and the industry begins alliance and cooperation or reorganization and merger to rapidly enhance market concentration. [23]

Beyond the third stage, it is the whale swallowing of the Big Macs, and the concentration is increasing with each passing day. For example, such as BASF's acquisition of Merck's electronic chemistry business in 2004 [24] and Merck's merger and acquisition of Versum Materials in 2019. [25]

At present, China is still in the stage of development, compared with the century-old stores in the world, it is difficult to achieve large-scale integration and mergers and acquisitions at this stage, so it may be a good way to develop around the industrial chain.

Upstream, raw material prices and supply are the lifeline of wet electronic chemical production enterprises, refinery shutdown will affect the cost and availability of isopropanol and sulfuric acid, with stricter environmental control, raw material price fluctuations also affect product production, in addition, the rise and restriction of natural gas and oil prices for power generation in manufacturing will lead to a rise in chemical prices.

For example, hydrofluoric acid is generally made by adding sulfuric acid to fluorite, while 60% of the fluorite with an annual output of 7 million tons in the world is produced in China, resulting in more than 90% of Japan's hydrofluoric acid and its main raw materials imported from China [26]. China's polyfluorine, Xingfu Electronics, Binhua, SMIC and other enterprises all have G5 hydrofluoric acid, which not only enters the international industrial chain of TSMC and SMIC. It has also become the main substitute in the semiconductor trade war between Japan and South Korea.

In the middle and lower reaches, the cost of packaging and transportation of wet electronic chemicals as hazardous chemicals is extremely high, so most manufacturers of wet electronic chemicals build factories around chip manufacturers.

For example, after TSMC announced plans to build a plant in Arizona, its supplier LCY announced plans to repackage and purify isopropanol in Arizona, while another supplier, Changchun Chemical, followed suit by producing electronic-grade hydrogen peroxide and tetramethyl ammonium hydroxide-based developers, electronic-grade solutions and plating baths in Arizona. [12]

It can be said that although there is still a gap in domestic wet electronic chemicals, there is an adequate supply of upstream raw materials, which brings great advantages for domestic production enterprises, and the rest is to increase their own thickness around the industrial chain.

As the nano-process is getting closer and closer to 1nm, the process differences among chip manufacturers are increasing, and the demand for customized wet electronic chemicals is increasing, which may become a turning point for domestic enterprises.

References:

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[17] Jin Hainian, etc. The ridge of a big country: how to solve the problem of "neck jam". Chinese Translation Press [M], 2022.3

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[21] SIA:Comments of the Semiconductor Industry Association (SIA) On the CHIPS Program Office Request for Information On Implementation of the CHIPS Incentives Program.2022.11.14. https://www.semiconductors.org/wp-content/uploads/2022/11/SIA-CPO-CHIPS-RFI-Response-11_14_22.pdf

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[26] Nikkei Chinese website: Daijin new technology to get rid of dependence on hydrofluoric acid raw materials produced in China. 2022.3.9. Https://cn.nikkei.com/ industry / manufacturing / 47868-2022-03-09-09-05-28.html

This article comes from the official account of Wechat: fruit Shell hard Technology (ID:guokr233), author: Fu Bin

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