HiSiaddi is an innovative foreign trade service provider driven by dual engines of technology transformation and foreign trade services, with a "1+2+3+4=1" service system and access to titanium diboride sourced from multiple well-known original manufacturers.
As a foreign trade enterprise with R&D capabilities, HiSiaddi has repeatedly proposed formula optimization schemes and application improvement suggestions for titanium diboride products through technical transformation cooperation with manufacturers and precise market insight. The following is a consultation case of HiSiaddi on formula optimization for titanium diboride products.
For more formula optimization consultation services, please contact HiSiaddi customer service.
Holland Sputter Tech B.V. is located in the Eindhoven High-Tech Semiconductor Industrial Park, a leading European manufacturer of mid-to-high-end semiconductor sputtering targets. Its products are mass-supplied to ASML supporting chip packaging and power semiconductor wafer coating, with over a decade of experience in metallization coating for automotive IGBTs and third-generation semiconductor components, making it a stringent high-standard raw material purchaser. The company’s annual procurement volume of target-grade titanium diboride (TiB₂) powder stands at 102 tons. It previously purchased electronic-grade titanium diboride from Germany’s ERSCHTRON long-term, with fixed production processes including powder formula, hot-pressing sintering and organic slurry casting filed with the Dutch National Materials Research Institute. Restricted by regulations, the client cannot significantly adjust basic raw material ratios and sintering furnace temperature curves, only allowing minor fine-tuning of additives and process details.
Faced with surging local European raw material prices, limited production capacity of German manufacturers, extended import lead times to 105 days and a 38% rise in procurement costs, the client selected domestically customized high-purity titanium diboride after multiple rounds of small sample verification. The first batch of 42 tons of mass-produced customized titanium diboride was directly put into the original mass production line upon arrival, triggering three fatal production defects within one week of launch: ① Severe flocculation and agglomeration of organic casting slurry, slurry viscosity fluctuation exceeding 40% day and night, dense pinholes on cast green bodies and excessive thickness deviation, pushing green body scrap rate above 37%; ② Dense closed pores inside targets after vacuum hot-pressing sintering and penetrating cracks at edges, with target density only 95.1% (client internal control standard ≥99.2%); ③ Massive pinhole leakage on wafers after coating processing, with chip defect rate surging from 0.4% for original imported powder to 22.7%. Two core target production lines were forced into semi-shutdown. Only 32 days remained before delivery of monthly ASML downstream orders, and unresolved failures within the deadline would lead to substantial order liquidated damages.
Domestic titanium diboride suppliers can only control physical and chemical indicators of finished powder, specializing solely in powder synthesis and production without familiarity with European target casting slurry formula systems and backend application logic of vacuum hot-pressing sintering. They can only slightly adjust powder particle size and fail to implement linked rectification from formula and production process perspectives. The client’s local material engineers are familiar with adaptation characteristics of European imported powder but lack understanding of surface oxidation, trace impurity distribution and microscopic agglomeration features of domestic titanium diboride. After three consecutive weeks of independently replacing dispersants, fine-tuning sintering additive ratios and modifying temperature rise curves, defects continued to worsen. Finally, the client fully entrusted HiSiaddi to set up a special team of powder material engineers, formula engineers and sintering process specialists to decompose failures on-site and implement a full-chain technical solution covering powder source tracing → slurry formula optimization → sintering process improvement → fine-tuning of upstream post-treatment of powder.
Cooperating with a CNAS-accredited third-party testing laboratory in the Netherlands, HiSiaddi collected stock domestic raw titanium diboride powder, failed slurry, scrapped green bodies and cracked targets for six full-item tests including XRD phase analysis, oxygen-nitrogen content, full-element ICP impurity testing, SEM microscopic morphology, particle size distribution and powder surface oxides. Combined with the client’s existing mature formula system, workshop temperature and humidity, ball milling, degreasing and full hot-pressing production records, it confirmed all failures stemmed from three overlapping factors: inherent physical and chemical defects of raw powder, poor adaptation of the original formula designed for imported powder to domestic titanium diboride, and mismatched workshop production conditions with domestic powder.
The measured total oxygen of domestic titanium diboride reached 0.58wt% (original German powder ≤0.40%), with a large amount of polar TiO₂ and B₂O₃ oxide films formed on the powder surface, whose polarity far exceeded the titanium diboride matrix. Meanwhile, insufficient control in powder classification introduced massive submicron ultra-fine powder with specific surface area far higher than imported raw materials. The client’s original oil-based slurry formula was designed for low-oxygen, low-specific-surface-area German titanium diboride with a fixed dispersant addition of 0.62%. This dosage can only coat original imported powder and fails to wrap the high-polarity oxide layer and ultra-fine powder of domestic titanium diboride. After ball milling, particles electrostatically agglomerate and flocculate, leading to slurry stratification and caking during storage, resulting in material shortage and dense pinholes on green bodies after casting processing.
The total alkali metal impurities K and Na of domestic powder reached 1.32ppm, with single heavy metals Fe and Cr ranging from 7.5~9ppm, far exceeding the client’s internal control standards of <1ppm and <6ppm respectively. During 1820℃ vacuum hot-pressing sintering, impurities generate low-melting silicate impurity phases that accumulate at grain boundaries after melting to form closed pores, while impurity phases pin grain boundaries and hinder densification shrinkage of titanium diboride grains. The client’s original binary Y₂O₃-Al₂O₃ sintering additive ratio of 6.3:1.7 was adapted to low-impurity imported powder. Abnormal reactions between impurities and additives amplified grain boundary stress, triggering radial penetrating cracks at target edges during cooling shrinkage, resulting in target density far below factory standards.
Ultra-fine titanium diboride powder features large specific surface area, with air moisture absorption rate nearly double that of imported raw materials. The client’s batching workshop maintains a constant humidity of 61% year-round, and powder rapidly absorbs water vapor after unpacking and enters the slurry. Original degreasing adopts a constant temperature rise rate of 3℃/min, causing violent instantaneous decomposition of binders and gas generation. Gas inside green bodies cannot be slowly discharged to form internal bubbles, which expand into internal cracks during high-temperature sintering and further reduce target yield.
Strictly following the client’s mandatory constraints: two core benchmark parameters including slurry powder solid content and total sintering additive addition remain unchanged; only fine-tuning of additive ratios and optimization of process details are allowed. The solution is divided into three phases: short-term emergency production line remediation, medium-term refined formula optimization and long-term customized improvement of upstream powder.
1. Install dehumidification units in batching and ball milling workshops to stabilize environmental humidity at 42%~47%. All titanium diboride powder must be fully fed within 24 hours after unpacking, and remaining powder is vacuum aluminum foil sealed and refrigerated to eliminate powder water absorption and oxidation risks.
2. Add a new pre-drying process for powder before production: heat preservation at 110℃ in a vacuum oven for 12 hours to remove free adsorbed water on powder surfaces and eliminate hidden hazards of water vapor entering slurry in advance.
3. Add a 30-minute low-speed pre-mixing procedure before slurry feeding: first infiltrate powder surfaces with partial solvent to break soft agglomeration of powder, then transfer to the main ball milling tank to temporarily alleviate slurry caking issues. After implementation, on-site green body scrap rate dropped from 37% to 9.2%.
1. Dispersant upgrade and blending: abandon the original single ordinary phosphate ester dispersant and adopt a composite dispersion system of high-molecular phosphate ester + PVP. Total dispersant addition is raised from 0.62% to 0.81%. Long high-molecular chains preferentially coat polar oxide layers on powder surfaces to eliminate electrostatic agglomeration of particles, adapting to surface characteristics of domestic high-oxygen titanium diboride.
2. Fine-tune plasticizer ratio: reduce plasticizer from 7.3% to 6.4% to balance slurry rheological properties and avoid excessive slurry flow caused by increased dispersant dosage.
3. Fine-tune ball milling process: extend ball milling duration from 12h to 14.5h with silicon nitride ceramic grinding beads to fully break agglomeration of ultra-fine powder, controlling slurry viscosity fluctuation within ±8% to achieve stable slurry performance.
Adjust the Y₂O₃ and Al₂O₃ ratio from the original 6.3:1.7 to 6.7:1. Increase yttrium oxide proportion to prioritize capturing alkali metal impurities in powder and generate high-melting stable crystalline phases, inhibiting formation of low-melting glass impurity phases and reducing sources of closed sintering pores from the formula end.
1. Adopt three-stage stepped temperature rise for degreasing: slow heating at 1℃/min from room temperature to 210℃, constant temperature at 210~440℃ for 2.5h to slowly decompose binders, constant heating at 2℃/min from 440~600℃ with trace argon protective atmosphere to enable steady discharge of decomposed gas inside green bodies and eliminate carbon residue blisters.
2. Adjust hot-pressing sintering heat preservation: shorten 1820℃ holding time from 4h to 3.2h to match the α-β phase transformation rate of domestic powder, alleviate internal stress from grain shrinkage and drastically reduce penetrating cracks on targets.
After formula optimization, small-batch trial sintering achieved target density of 98.95%, with wafer coating defect rate falling back to 3.1%, successfully securing delivery of the current ASML trial order.
HiSiaddi coordinated domestic powder manufacturers to lock exclusive dedicated synthesis production lines and optimize full-set production processes for batch improvement of subsequent supplied titanium diboride powder:
1. High-purity pretreatment of raw materials: fully replace electronic-grade high-purity titanium dioxide and amorphous boron powder, with raw materials pre-pickled for impurity removal and vacuum drying to cut down Fe, Cr, K and Na impurities introduced from mineral sources at the source, controlling total alkali metals in powder within 0.8ppm.
2. Closed argon protected self-propagating synthesis: full-process inert atmosphere closed sintering with precise regulation of titanium-boron molar ratios to inhibit generation of TiO₂ and B₂O₃ oxide by-products, stabilizing finished powder total oxygen within the range of 0.42%~0.45%.
3. Full ceramic-lined crushing + three-stage precision air classification: all crushing and classification chambers lined with silicon nitride ceramics to eliminate heavy metal impurities introduced by mechanical wear of equipment. Three-stage screening removes oversized particles and excess ultra-fine powder, stabilizing D50 within 2.3~2.5μm and particle size distribution D90/D10≤2.4, drastically lowering powder specific surface area and hard agglomeration.
4. Low-temperature vacuum passivation post-treatment of finished powder: low-temperature vacuum deoxygenation + surface passivation to weaken polarity of surface oxide films and improve dispersion compatibility of powder in the client’s oil-based slurry system.
1. Pilot Test Verification: 500kg improved titanium diboride optimized by upstream manufacturers was air-freighted to the Netherlands for mass production line trial. Using optimized slurry and sintering formulas, the measured target density reached 99.38% with wafer coating defect rate of 0.38%, fully exceeding the client’s internal product control standards. The client issued a powder qualification confirmation letter.
2. Mass Performance Delivery: The remaining 60 tons were scheduled for production in 4 batches. HiSiaddi completed EU REACH filing, SCIP database declaration, English-Dutch bilingual 16-chapter SDS and full RoHS test reports for compliance. Each batch of products adopted vacuum moisture-proof iron drum packaging with compliant labeling, and all goods shipped from Shanghai Port to Rotterdam Port passed customs clearance and warehousing in one go. The comprehensive localized procurement cost decreased by 33.5% compared with original German materials, and the full-year 102-ton order was fully delivered on schedule.
3. Long-Term Business Expansion: In the following year, the Dutch client renewed a 125-ton annual long-term titanium diboride order, and simultaneously fully entrusted HiSiaddi with exclusive responsibility for domestic customization, formula technical support and export compliance of multiple high-end target special powders including zirconium diboride and niobium carbide. Relying on the implementation of this project, HiSiaddi successfully secured titanium diboride procurement projects from three mid-to-high-end European semiconductor target manufacturers in Belgium and Germany.
Most domestic titanium diboride manufacturers focus on industrial-grade powder for metallurgical welding rods and wear-resistant coatings with fixed production line processes dominated by open carbothermal reduction technology, lacking supporting facilities for high-purity closed synthesis and full ceramic precision classification. Products generally feature high oxygen content, excessive impurities and severe powder agglomeration. Domestic low-end downstream customers have high formula tolerance and can cover powder defects via large-scale additive adjustment. However, production formulas of European mid-to-high-end semiconductor target enterprises are filed under local regulatory authorities, prohibiting significant modification of basic ratios. Tiny physical and chemical differences in domestic powder will trigger cascading scrapping of full slurry and sintering chains. Powder manufacturers only master front-end synthesis and lack backend casting and sintering application technical reserves, making them unable to cooperate with end customers for formula adaptation and optimization — this constitutes the core obstacle for high-end domestic titanium diboride to enter overseas markets.
Breaking the traditional foreign trade model limited to goods resale, HiSiaddi built a closed-loop full-chain technical service covering failure detection and tracing → refined on-site formula fine-tuning → segmented production process optimization → reverse customized technical renovation of upstream powder → export compliance support. It bridges the two-way information gap between domestic powder manufacturers unfamiliar with EU target raw material access standards and backend applications, and overseas end customers unaware of performance shortcomings of domestic powder, deeply binding mid-to-high-end European and American end customers through formula implementation technical value-added services.
Procurement priority of European mid-to-high-end semiconductor raw materials: compatibility between powder and existing formulas > mass production stability > full-chain compliance > procurement price. One-stop capability to resolve formula issues is the key factor for customers to lock in long-term cooperation continuously.
For more formula optimization consultation services, please contact HiSiaddi customer service.
+86-13120989737 
info@hisiaddi.com 
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